# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1631 data_L3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common L3 _chemical_formula_moiety ? _chemical_formula_sum 'C21 H26 N2 O2' _chemical_formula_weight 338.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 8.910(12) _cell_length_b 26.75(3) _cell_length_c 9.245(9) _cell_angle_alpha 90.00 _cell_angle_beta 117.610(10) _cell_angle_gamma 90.00 _cell_volume 1952(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.074 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4290 _diffrn_reflns_av_R_equivalents 0.0194 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 24.92 _reflns_number_total 2636 _reflns_number_gt 2034 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0884P)^2^+0.4066P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.049(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2636 _refine_ls_number_parameters 230 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1465 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C12 C 0.4170(3) 0.54752(10) 0.3139(3) 0.0797(8) Uani 1 d . . . H12A H 0.4440 0.5129 0.3403 0.120 Uiso 1 calc R . . H12B H 0.4299 0.5558 0.2192 0.120 Uiso 1 calc R . . H12C H 0.3022 0.5536 0.2918 0.120 Uiso 1 calc R . . N11 N 0.5313(2) 0.57845(6) 0.4514(2) 0.0562(5) Uani 1 d . . . C13 C 0.6857(3) 0.59462(7) 0.4525(3) 0.0508(6) Uani 1 d . . . C14 C 0.8274(3) 0.56487(8) 0.5213(3) 0.0630(7) Uani 1 d . . . H14 H 0.8244 0.5348 0.5706 0.076 Uiso 1 calc R . . C15 C 0.9742(3) 0.57929(9) 0.5176(3) 0.0696(7) Uani 1 d . . . H15 H 1.0703 0.5592 0.5659 0.083 Uiso 1 calc R . . C16 C 0.9789(3) 0.62304(10) 0.4431(3) 0.0694(7) Uani 1 d . . . H16 H 1.0779 0.6327 0.4406 0.083 Uiso 1 calc R . . C17 C 0.8373(3) 0.65255(10) 0.3722(4) 0.0725(7) Uani 1 d . . . H17 H 0.8404 0.6822 0.3211 0.087 Uiso 1 calc R . . C18 C 0.6893(3) 0.63842(8) 0.3761(3) 0.0623(7) Uani 1 d . . . H18 H 0.5932 0.6584 0.3274 0.075 Uiso 1 calc R . . C2 C 0.4851(2) 0.59065(8) 0.5675(3) 0.0558(6) Uani 1 d . . . O1 O 0.35326(19) 0.57433(7) 0.5605(2) 0.0815(6) Uani 1 d . . . C3 C 0.6034(2) 0.62468(7) 0.7052(3) 0.0514(6) Uani 1 d . . . H3 H 0.7201 0.6134 0.7421 0.062 Uiso 1 calc R . . C31 C 0.5654(3) 0.62352(9) 0.8511(3) 0.0664(7) Uani 1 d . . . H31A H 0.6283 0.6502 0.9258 0.080 Uiso 1 calc R . . H31B H 0.4458 0.6302 0.8120 0.080 Uiso 1 calc R . . C32 C 0.6096(4) 0.57423(9) 0.9445(4) 0.0761(8) Uani 1 d . . . H32A H 0.5825 0.5770 1.0344 0.091 Uiso 1 calc R . . H32B H 0.5382 0.5482 0.8723 0.091 Uiso 1 calc R . . C33 C 0.7899(4) 0.55837(12) 1.0110(4) 0.0950(10) Uani 1 d . . . H33A H 0.8622 0.5855 1.0756 0.114 Uiso 1 calc R . . H33B H 0.8145 0.5524 0.9206 0.114 Uiso 1 calc R . . C34 C 0.8332(5) 0.51159(13) 1.1161(5) 0.1248(14) Uani 1 d . . . H34A H 0.9514 0.5041 1.1575 0.187 Uiso 1 calc R . . H34B H 0.7669 0.4840 1.0515 0.187 Uiso 1 calc R . . H34C H 0.8088 0.5171 1.2056 0.187 Uiso 1 calc R . . C4 C 0.5861(3) 0.67770(8) 0.6395(3) 0.0543(6) Uani 1 d . . . O5 O 0.4552(2) 0.69073(6) 0.5196(2) 0.0741(6) Uani 1 d . . . N21 N 0.7155(2) 0.70982(6) 0.7177(2) 0.0602(6) Uani 1 d . . . C23 C 0.8710(3) 0.69793(8) 0.8600(3) 0.0589(6) Uani 1 d . . . C24 C 0.9879(3) 0.66643(9) 0.8496(3) 0.0675(7) Uani 1 d . . . H24 H 0.9665 0.6527 0.7494 0.081 Uiso 1 calc R . . C25 C 1.1373(4) 0.65508(13) 0.9878(5) 0.0941(10) Uani 1 d . . . H25 H 1.2139 0.6328 0.9810 0.113 Uiso 1 calc R . . C26 C 1.1718(5) 0.67641(18) 1.1330(5) 0.1130(13) Uani 1 d . . . H26 H 1.2726 0.6689 1.2252 0.136 Uiso 1 calc R . . C27 C 1.0606(6) 0.70867(16) 1.1450(4) 0.1059(12) Uani 1 d . . . H27 H 1.0865 0.7234 1.2450 0.127 Uiso 1 calc R . . C28 C 0.9069(4) 0.72008(11) 1.0079(4) 0.0843(9) Uani 1 d . . . H28 H 0.8305 0.7421 1.0162 0.101 Uiso 1 calc R . . C22 C 0.6962(4) 0.76110(9) 0.6543(4) 0.0836(8) Uani 1 d . . . H22A H 0.7334 0.7625 0.5721 0.125 Uiso 1 calc R . . H22B H 0.7633 0.7835 0.7418 0.125 Uiso 1 calc R . . H22C H 0.5793 0.7708 0.6076 0.125 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C12 0.0782(18) 0.0786(16) 0.070(2) -0.0196(14) 0.0241(16) -0.0249(13) N11 0.0493(10) 0.0618(11) 0.0561(13) -0.0105(9) 0.0233(10) -0.0102(8) C13 0.0511(12) 0.0559(11) 0.0485(15) -0.0083(10) 0.0258(12) -0.0032(9) C14 0.0654(15) 0.0600(13) 0.0712(19) 0.0053(11) 0.0381(14) 0.0079(10) C15 0.0584(14) 0.0778(16) 0.080(2) 0.0000(13) 0.0387(15) 0.0118(11) C16 0.0629(15) 0.0832(16) 0.0764(19) -0.0034(14) 0.0443(14) -0.0025(12) C17 0.0764(16) 0.0724(15) 0.081(2) 0.0080(13) 0.0469(15) -0.0018(12) C18 0.0566(13) 0.0687(14) 0.0612(17) 0.0059(12) 0.0271(13) 0.0058(10) C2 0.0378(11) 0.0636(13) 0.0612(17) 0.0000(11) 0.0189(12) -0.0006(9) O1 0.0446(9) 0.1102(14) 0.0929(16) -0.0102(10) 0.0346(10) -0.0166(8) C3 0.0424(11) 0.0584(12) 0.0546(15) 0.0006(10) 0.0235(11) 0.0037(8) C31 0.0718(15) 0.0729(14) 0.0661(18) -0.0046(12) 0.0418(14) 0.0004(11) C32 0.104(2) 0.0717(16) 0.0688(19) -0.0037(13) 0.0535(18) -0.0099(14) C33 0.107(2) 0.095(2) 0.072(2) 0.0212(16) 0.033(2) 0.0128(17) C34 0.172(4) 0.100(2) 0.080(3) 0.0241(19) 0.039(3) 0.020(2) C4 0.0499(13) 0.0616(12) 0.0502(16) 0.0008(11) 0.0223(13) 0.0115(10) O5 0.0590(10) 0.0826(11) 0.0631(13) 0.0045(9) 0.0133(10) 0.0222(8) N21 0.0638(12) 0.0542(10) 0.0599(14) 0.0052(9) 0.0264(12) 0.0022(8) C23 0.0631(14) 0.0623(13) 0.0496(16) -0.0018(11) 0.0247(13) -0.0141(10) C24 0.0509(14) 0.0864(16) 0.0580(18) 0.0035(13) 0.0190(15) -0.0052(11) C25 0.0571(18) 0.122(2) 0.086(3) 0.018(2) 0.018(2) -0.0042(15) C26 0.078(2) 0.161(4) 0.076(3) 0.022(3) 0.015(2) -0.036(2) C27 0.116(3) 0.141(3) 0.049(2) -0.017(2) 0.028(2) -0.064(2) C28 0.101(2) 0.0913(19) 0.065(2) -0.0138(15) 0.042(2) -0.0269(16) C22 0.104(2) 0.0613(14) 0.090(2) 0.0144(14) 0.0498(19) 0.0040(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C12 N11 1.462(3) . ? N11 C2 1.355(3) . ? N11 C13 1.438(3) . ? C13 C14 1.374(3) . ? C13 C18 1.376(3) . ? C14 C15 1.379(4) . ? C15 C16 1.368(4) . ? C16 C17 1.370(4) . ? C17 C18 1.389(4) . ? C2 O1 1.226(3) . ? C2 C3 1.522(3) . ? C3 C4 1.522(3) . ? C3 C31 1.535(4) . ? C31 C32 1.524(4) . ? C32 C33 1.491(4) . ? C33 C34 1.520(4) . ? C4 O5 1.230(3) . ? C4 N21 1.348(3) . ? N21 C23 1.436(3) . ? N21 C22 1.470(3) . ? C23 C24 1.377(4) . ? C23 C28 1.385(4) . ? C24 C25 1.385(4) . ? C25 C26 1.356(5) . ? C26 C27 1.357(5) . ? C27 C28 1.402(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N11 C13 124.26(18) . . ? C2 N11 C12 118.7(2) . . ? C13 N11 C12 117.0(2) . . ? C14 C13 C18 119.7(2) . . ? C14 C13 N11 120.0(2) . . ? C18 C13 N11 120.14(19) . . ? C13 C14 C15 120.3(2) . . ? C16 C15 C14 120.1(2) . . ? C15 C16 C17 119.9(2) . . ? C16 C17 C18 120.3(2) . . ? C13 C18 C17 119.6(2) . . ? O1 C2 N11 120.5(2) . . ? O1 C2 C3 122.1(2) . . ? N11 C2 C3 117.37(19) . . ? C4 C3 C2 108.68(19) . . ? C4 C3 C31 110.32(17) . . ? C2 C3 C31 111.94(19) . . ? C32 C31 C3 114.25(19) . . ? C33 C32 C31 115.2(2) . . ? C32 C33 C34 113.8(3) . . ? O5 C4 N21 121.4(2) . . ? O5 C4 C3 120.1(2) . . ? N21 C4 C3 118.5(2) . . ? C4 N21 C23 124.90(19) . . ? C4 N21 C22 117.9(2) . . ? C23 N21 C22 117.2(2) . . ? C24 C23 C28 119.6(3) . . ? C24 C23 N21 120.8(2) . . ? C28 C23 N21 119.5(2) . . ? C23 C24 C25 120.3(3) . . ? C26 C25 C24 120.1(4) . . ? C25 C26 C27 120.6(4) . . ? C26 C27 C28 120.6(4) . . ? C23 C28 C27 118.8(3) . . ? _refine_diff_density_max 0.157 _refine_diff_density_min -0.172 _refine_diff_density_rms 0.037 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_L4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety L4 _chemical_formula_sum 'C21 H26 N2 O3 ' _chemical_formula_weight 354.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.080(9) _cell_length_b 9.666(12) _cell_length_c 13.158(14) _cell_angle_alpha 76.504(10) _cell_angle_beta 81.190(10) _cell_angle_gamma 61.322(10) _cell_volume 984.1(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3463 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3463 _reflns_number_gt 2417 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1057P)^2^+0.1865P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.069(9) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3463 _refine_ls_number_parameters 239 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1837 _refine_ls_wR_factor_gt 0.1641 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.121 _refine_ls_shift/su_mean 0.028 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.77764(19) 0.45016(18) 0.14714(13) 0.0569(5) Uani 1 d . . . C2 C 0.9127(2) 0.4118(2) 0.18137(16) 0.0400(5) Uani 1 d . . . C3 C 1.0125(2) 0.2467(2) 0.24770(15) 0.0401(5) Uani 1 d . . . H3 H 1.1306 0.2024 0.2225 0.048 Uiso 1 calc R . . C4 C 1.0003(3) 0.2636(2) 0.36106(16) 0.0459(5) Uani 1 d . . . O5 O 0.8715(2) 0.3679(2) 0.39664(13) 0.0645(5) Uani 1 d . . . N11 N 0.9813(2) 0.51375(19) 0.15914(13) 0.0416(4) Uani 1 d . . . C12 C 0.8919(3) 0.6708(3) 0.0919(2) 0.0561(6) Uani 1 d . . . H12A H 0.8165 0.6665 0.0503 0.067 Uiso 1 calc R . . H12B H 0.9716 0.6977 0.0467 0.067 Uiso 1 calc R . . H12C H 0.8290 0.7509 0.1346 0.067 Uiso 1 calc R . . C13 C 1.1352(2) 0.4839(2) 0.19840(16) 0.0402(5) Uani 1 d . . . C14 C 1.2810(3) 0.4430(3) 0.13349(18) 0.0494(6) Uani 1 d . . . H14 H 1.2814 0.4273 0.0663 0.059 Uiso 1 calc R . . C15 C 1.4247(3) 0.4262(3) 0.1697(2) 0.0572(6) Uani 1 d . . . H15 H 1.5218 0.3993 0.1264 0.069 Uiso 1 calc R . . C16 C 1.4262(3) 0.4486(3) 0.2690(2) 0.0599(7) Uani 1 d . . . H16 H 1.5240 0.4363 0.2927 0.072 Uiso 1 calc R . . C17 C 1.2816(3) 0.4896(3) 0.3335(2) 0.0603(6) Uani 1 d . . . H17 H 1.2823 0.5041 0.4008 0.072 Uiso 1 calc R . . C18 C 1.1359(3) 0.5091(3) 0.29759(18) 0.0496(6) Uani 1 d . . . H18 H 1.0381 0.5392 0.3403 0.060 Uiso 1 calc R . . N21 N 1.1309(2) 0.1592(2) 0.42254(14) 0.0551(5) Uani 1 d . . . C22 C 1.1202(4) 0.1844(4) 0.5304(2) 0.0822(9) Uani 1 d . . . H22A H 1.1423 0.2725 0.5290 0.099 Uiso 1 calc R . . H22B H 1.2017 0.0891 0.5712 0.099 Uiso 1 calc R . . H22C H 1.0096 0.2082 0.5610 0.099 Uiso 1 calc R . . C23 C 1.2809(3) 0.0278(3) 0.39104(18) 0.0499(6) Uani 1 d . . . C24 C 1.3083(4) -0.1285(3) 0.4326(2) 0.0691(8) Uani 1 d . . . H24 H 1.2285 -0.1471 0.4787 0.083 Uiso 1 calc R . . C25 C 1.4566(5) -0.2571(3) 0.4046(3) 0.0871(11) Uani 1 d . . . H25 H 1.4764 -0.3617 0.4331 0.105 Uiso 1 calc R . . C26 C 1.5727(4) -0.2302(4) 0.3357(3) 0.0869(10) Uani 1 d . . . H26 H 1.6697 -0.3164 0.3159 0.104 Uiso 1 calc R . . C27 C 1.5467(4) -0.0771(3) 0.2958(3) 0.0765(8) Uani 1 d . . . H27 H 1.6266 -0.0596 0.2491 0.092 Uiso 1 calc R . . C28 C 1.4019(3) 0.0531(3) 0.3243(2) 0.0579(6) Uani 1 d . . . H28 H 1.3867 0.1570 0.2985 0.069 Uiso 1 calc R . . C31 C 0.9443(3) 0.1295(3) 0.24237(19) 0.0510(6) Uani 1 d . . . H31A H 1.0041 0.0301 0.2906 0.061 Uiso 1 calc R . . H31B H 0.8266 0.1754 0.2657 0.061 Uiso 1 calc R . . C32 C 0.9607(3) 0.0914(3) 0.1341(2) 0.0580(6) Uani 1 d . . . H32A H 0.9278 0.0080 0.1397 0.070 Uiso 1 calc R . . H32B H 0.8829 0.1863 0.0894 0.070 Uiso 1 calc R . . O33 O 1.1233(2) 0.04071(18) 0.08618(13) 0.0585(5) Uani 1 d . . . C34 C 1.2398(3) -0.1200(3) 0.1252(2) 0.0657(7) Uani 1 d . . . H34A H 1.1945 -0.1915 0.1220 0.079 Uiso 1 calc R . . H34B H 1.2598 -0.1309 0.1976 0.079 Uiso 1 calc R . . C35 C 1.3988(4) -0.1630(4) 0.0615(3) 0.0859(9) Uani 1 d . . . H35A H 1.3795 -0.1584 -0.0092 0.103 Uiso 1 calc R . . H35B H 1.4800 -0.2697 0.0899 0.103 Uiso 1 calc R . . H35C H 1.4405 -0.0889 0.0623 0.103 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0358(9) 0.0521(10) 0.0808(12) 0.0024(8) -0.0190(7) -0.0205(7) C2 0.0282(10) 0.0410(11) 0.0487(12) -0.0079(9) -0.0013(8) -0.0147(8) C3 0.0319(10) 0.0386(11) 0.0490(12) -0.0052(9) -0.0014(8) -0.0170(8) C4 0.0423(12) 0.0445(12) 0.0484(12) -0.0046(9) 0.0014(9) -0.0208(10) O5 0.0548(10) 0.0635(11) 0.0592(10) -0.0132(8) 0.0122(8) -0.0180(8) N11 0.0352(10) 0.0378(9) 0.0489(10) -0.0014(7) -0.0075(7) -0.0159(7) C12 0.0529(14) 0.0411(13) 0.0671(15) 0.0047(10) -0.0149(11) -0.0190(10) C13 0.0341(11) 0.0361(11) 0.0527(12) -0.0086(8) -0.0037(8) -0.0174(8) C14 0.0458(13) 0.0540(14) 0.0542(13) -0.0151(10) 0.0037(9) -0.0272(10) C15 0.0413(13) 0.0587(15) 0.0777(17) -0.0199(12) 0.0062(11) -0.0273(11) C16 0.0419(14) 0.0611(15) 0.0886(19) -0.0202(13) -0.0102(12) -0.0285(11) C17 0.0624(16) 0.0681(16) 0.0628(15) -0.0218(12) -0.0110(12) -0.0333(13) C18 0.0445(13) 0.0538(14) 0.0573(14) -0.0199(10) 0.0032(9) -0.0252(10) N21 0.0560(12) 0.0593(12) 0.0450(11) -0.0077(9) -0.0071(8) -0.0223(10) C22 0.096(2) 0.100(2) 0.0478(15) -0.0120(14) -0.0084(14) -0.0425(19) C23 0.0508(13) 0.0435(12) 0.0538(13) -0.0011(10) -0.0213(10) -0.0187(10) C24 0.086(2) 0.0591(17) 0.0703(17) 0.0125(12) -0.0331(14) -0.0424(15) C25 0.112(3) 0.0353(14) 0.109(3) 0.0047(14) -0.067(2) -0.0206(16) C26 0.068(2) 0.0566(19) 0.117(3) -0.0228(17) -0.0436(19) -0.0002(15) C27 0.0501(15) 0.0629(18) 0.102(2) -0.0177(15) -0.0140(14) -0.0106(13) C28 0.0469(14) 0.0451(13) 0.0757(17) -0.0044(11) -0.0135(11) -0.0165(10) C31 0.0450(13) 0.0454(13) 0.0654(15) -0.0029(10) -0.0053(10) -0.0257(10) C32 0.0578(15) 0.0467(13) 0.0747(17) -0.0095(11) -0.0177(12) -0.0248(11) O33 0.0655(11) 0.0438(9) 0.0617(10) -0.0061(7) -0.0094(8) -0.0217(8) C34 0.0642(17) 0.0474(14) 0.0793(18) -0.0067(12) -0.0113(13) -0.0208(12) C35 0.071(2) 0.074(2) 0.098(2) -0.0189(17) -0.0057(16) -0.0207(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.224(3) . ? C2 N11 1.358(3) . ? C2 C3 1.528(3) . ? C3 C4 1.520(3) . ? C3 C31 1.547(3) . ? C4 O5 1.234(3) . ? C4 N21 1.358(3) . ? N11 C13 1.437(3) . ? N11 C12 1.469(3) . ? C13 C18 1.384(3) . ? C13 C14 1.396(3) . ? C14 C15 1.381(4) . ? C15 C16 1.377(4) . ? C16 C17 1.384(4) . ? C17 C18 1.386(4) . ? N21 C23 1.432(3) . ? N21 C22 1.476(4) . ? C23 C28 1.378(4) . ? C23 C24 1.392(4) . ? C24 C25 1.397(5) . ? C25 C26 1.364(5) . ? C26 C27 1.365(5) . ? C27 C28 1.391(4) . ? C31 C32 1.521(4) . ? C32 O33 1.408(3) . ? O33 C34 1.418(3) . ? C34 C35 1.475(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C2 N11 120.90(19) . . ? O1 C2 C3 121.54(18) . . ? N11 C2 C3 117.53(18) . . ? C4 C3 C2 109.25(17) . . ? C4 C3 C31 108.52(16) . . ? C2 C3 C31 111.59(19) . . ? O5 C4 N21 121.1(2) . . ? O5 C4 C3 120.1(2) . . ? N21 C4 C3 118.76(18) . . ? C2 N11 C13 125.55(17) . . ? C2 N11 C12 118.85(19) . . ? C13 N11 C12 115.58(17) . . ? C18 C13 C14 119.6(2) . . ? C18 C13 N11 120.05(18) . . ? C14 C13 N11 120.1(2) . . ? C15 C14 C13 119.5(2) . . ? C16 C15 C14 120.9(2) . . ? C15 C16 C17 119.7(2) . . ? C16 C17 C18 119.9(2) . . ? C13 C18 C17 120.3(2) . . ? C4 N21 C23 125.56(19) . . ? C4 N21 C22 117.6(2) . . ? C23 N21 C22 116.8(2) . . ? C28 C23 C24 119.5(2) . . ? C28 C23 N21 121.2(2) . . ? C24 C23 N21 119.2(3) . . ? C23 C24 C25 119.5(3) . . ? C26 C25 C24 120.4(3) . . ? C27 C26 C25 120.1(3) . . ? C26 C27 C28 120.6(3) . . ? C23 C28 C27 119.8(3) . . ? C32 C31 C3 114.34(18) . . ? O33 C32 C31 114.34(19) . . ? C32 O33 C34 114.65(19) . . ? O33 C34 C35 109.2(2) . . ? _refine_diff_density_max 0.241 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.048 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Nd(L3)2(NO3)3 _chemical_formula_sum 'C42 H52 N7 Nd O13' _chemical_formula_weight 1007.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 26.48(3) _cell_length_b 9.833(12) _cell_length_c 18.58(2) _cell_angle_alpha 90 _cell_angle_beta 96.725(10) _cell_angle_gamma 90 _cell_volume 4805(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2068 _exptl_absorpt_coefficient_mu 1.147 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.43 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7521 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4354 _reflns_number_gt 3688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0709P)^2^+12.2832P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00042(18) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4354 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1333 _refine_ls_wR_factor_gt 0.1253 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.293 _refine_ls_shift/su_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd Nd 0.0000 0.10219(4) 0.2500 0.04717(17) Uani 1 d S . . O1 O -0.05504(19) -0.0996(4) 0.2348(2) 0.0748(13) Uani 1 d . . . C2 C -0.0838(2) -0.1653(5) 0.2688(3) 0.0575(13) Uani 1 d . . . C3 C -0.08235(19) -0.1583(5) 0.3506(3) 0.0491(11) Uani 1 d . . . H3 H -0.1156 -0.1836 0.3648 0.059 Uiso 1 calc R . . C4 C -0.06836(17) -0.0156(5) 0.3768(2) 0.0437(10) Uani 1 d . . . O5 O -0.02624(13) 0.0337(4) 0.36649(17) 0.0536(8) Uani 1 d . . . N11 N -0.10004(16) 0.0538(5) 0.4140(2) 0.0537(10) Uani 1 d . . . C12 C -0.0844(3) 0.1898(8) 0.4417(4) 0.090(2) Uani 1 d . . . H12A H -0.0617 0.1806 0.4856 0.108 Uiso 1 calc R . . H12B H -0.1139 0.2403 0.4513 0.108 Uiso 1 calc R . . H12C H -0.0674 0.2371 0.4062 0.108 Uiso 1 calc R . . C13 C -0.15105(19) 0.0121(6) 0.4233(3) 0.0524(12) Uani 1 d . . . C14 C -0.1598(3) -0.0503(9) 0.4872(3) 0.082(2) Uani 1 d . . . H14 H -0.1333 -0.0699 0.5230 0.099 Uiso 1 calc R . . C15 C -0.2101(3) -0.0830(10) 0.4962(4) 0.104(3) Uani 1 d . . . H15 H -0.2171 -0.1241 0.5390 0.124 Uiso 1 calc R . . C16 C -0.2487(3) -0.0562(10) 0.4439(5) 0.097(2) Uani 1 d . . . H16 H -0.2818 -0.0804 0.4507 0.116 Uiso 1 calc R . . C17 C -0.2394(3) 0.0070(8) 0.3802(4) 0.084(2) Uani 1 d . . . H17 H -0.2661 0.0267 0.3446 0.101 Uiso 1 calc R . . C18 C -0.1901(2) 0.0406(6) 0.3700(3) 0.0636(14) Uani 1 d . . . H18 H -0.1834 0.0824 0.3272 0.076 Uiso 1 calc R . . N21 N -0.1181(2) -0.2496(5) 0.2314(3) 0.0714(14) Uani 1 d . . . C22 C -0.1177(4) -0.2618(10) 0.1523(4) 0.134(4) Uani 1 d . . . H22A H -0.1514 -0.2818 0.1299 0.161 Uiso 1 calc R . . H22B H -0.0952 -0.3338 0.1421 0.161 Uiso 1 calc R . . H22C H -0.1063 -0.1778 0.1334 0.161 Uiso 1 calc R . . C23 C -0.1522(2) -0.3377(6) 0.2644(3) 0.0592(13) Uani 1 d . . . C24 C -0.1966(2) -0.2890(7) 0.2850(3) 0.0692(15) Uani 1 d . . . H24 H -0.2050 -0.1975 0.2790 0.083 Uiso 1 calc R . . C25 C -0.2295(3) -0.3786(11) 0.3152(4) 0.097(3) Uani 1 d . . . H25 H -0.2599 -0.3471 0.3295 0.117 Uiso 1 calc R . . C26 C -0.2166(4) -0.5133(12) 0.3238(5) 0.111(3) Uani 1 d . . . H26 H -0.2381 -0.5726 0.3447 0.133 Uiso 1 calc R . . C27 C -0.1728(4) -0.5607(8) 0.3020(5) 0.102(3) Uani 1 d . . . H27 H -0.1647 -0.6524 0.3072 0.122 Uiso 1 calc R . . C28 C -0.1406(3) -0.4740(7) 0.2725(4) 0.0778(18) Uani 1 d . . . H28 H -0.1106 -0.5071 0.2577 0.093 Uiso 1 calc R . . N33 N 0.0000 0.4048(8) 0.2500 0.081(2) Uani 1 d S . . O34 O 0.0000 0.5302(8) 0.2500 0.153(4) Uani 1 d S . . O31 O 0.0030(2) 0.3389(5) 0.1933(3) 0.0948(15) Uani 1 d . . . N43 N 0.10726(18) 0.1654(7) 0.3147(3) 0.0829(17) Uani 1 d . . . O44 O 0.15122(18) 0.1868(12) 0.3399(3) 0.160(4) Uani 1 d . . . O41 O 0.09345(16) 0.1757(5) 0.2477(2) 0.0775(12) Uani 1 d . . . O42 O 0.07418(15) 0.1336(6) 0.3539(2) 0.0822(14) Uani 1 d . . . C31 C -0.0413(2) -0.2597(6) 0.3840(4) 0.0734(16) Uani 1 d . . . H31A H -0.0434 -0.3422 0.3552 0.088 Uiso 1 calc R . . H31B H -0.0079 -0.2201 0.3817 0.088 Uiso 1 calc R . . C32 C -0.0465(3) -0.2965(8) 0.4620(4) 0.092(2) Uani 1 d . . . H32A H -0.0520 -0.2143 0.4889 0.111 Uiso 1 calc R . . H32B H -0.0152 -0.3379 0.4839 0.111 Uiso 1 calc R . . C33 C -0.0906(4) -0.3944(10) 0.4674(6) 0.127(4) Uani 1 d . . . H33A H -0.1222 -0.3461 0.4538 0.153 Uiso 1 calc R . . H33B H -0.0885 -0.4668 0.4325 0.153 Uiso 1 calc R . . C34 C -0.0927(5) -0.4535(12) 0.5361(7) 0.155(5) Uani 1 d . . . H34A H -0.1188 -0.5219 0.5327 0.186 Uiso 1 calc R . . H34B H -0.1002 -0.3846 0.5698 0.186 Uiso 1 calc R . . H34C H -0.0605 -0.4943 0.5525 0.186 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd 0.0481(2) 0.0518(3) 0.0434(2) 0.000 0.01281(15) 0.000 O1 0.106(3) 0.070(3) 0.055(2) -0.0173(19) 0.038(2) -0.035(2) C2 0.072(3) 0.051(3) 0.053(3) -0.015(2) 0.019(3) -0.009(3) C3 0.057(3) 0.047(3) 0.045(3) -0.001(2) 0.016(2) -0.006(2) C4 0.047(2) 0.054(3) 0.031(2) 0.0009(19) 0.0054(18) -0.005(2) O5 0.060(2) 0.063(2) 0.0398(17) -0.0011(15) 0.0127(15) -0.0115(17) N11 0.057(2) 0.062(3) 0.044(2) -0.0154(19) 0.0156(19) -0.013(2) C12 0.090(5) 0.088(5) 0.097(5) -0.052(4) 0.035(4) -0.023(4) C13 0.052(3) 0.065(3) 0.042(3) -0.005(2) 0.015(2) -0.001(2) C14 0.066(4) 0.130(6) 0.052(3) 0.012(4) 0.016(3) -0.009(4) C15 0.083(5) 0.169(9) 0.064(4) 0.022(5) 0.031(4) -0.017(5) C16 0.057(4) 0.141(7) 0.096(5) -0.010(5) 0.028(4) -0.006(4) C17 0.065(4) 0.105(5) 0.080(5) -0.009(4) 0.004(3) 0.016(4) C18 0.067(4) 0.067(3) 0.057(3) 0.000(3) 0.007(3) 0.006(3) N21 0.084(3) 0.079(3) 0.056(3) -0.026(2) 0.027(2) -0.029(3) C22 0.184(10) 0.164(9) 0.062(4) -0.058(5) 0.053(5) -0.097(8) C23 0.060(3) 0.055(3) 0.063(3) -0.017(2) 0.007(3) -0.011(2) C24 0.061(3) 0.077(4) 0.068(4) -0.012(3) 0.004(3) 0.007(3) C25 0.052(4) 0.157(9) 0.085(5) -0.023(5) 0.017(3) -0.021(4) C26 0.123(8) 0.126(8) 0.082(5) 0.001(5) 0.004(5) -0.072(7) C27 0.114(7) 0.062(4) 0.120(7) 0.008(4) -0.018(6) -0.023(4) C28 0.068(4) 0.062(4) 0.101(5) -0.012(3) -0.001(3) -0.007(3) N33 0.068(5) 0.062(5) 0.119(7) 0.000 0.034(5) 0.000 O34 0.187(10) 0.050(5) 0.238(13) 0.000 0.102(9) 0.000 O31 0.130(4) 0.072(3) 0.087(3) 0.016(3) 0.030(3) 0.011(3) N43 0.043(3) 0.142(5) 0.062(3) 0.005(3) 0.000(2) 0.000(3) O44 0.044(3) 0.342(11) 0.090(4) 0.031(6) -0.009(2) -0.028(4) O41 0.063(2) 0.116(4) 0.053(2) 0.011(2) 0.0057(18) -0.012(2) O42 0.048(2) 0.148(4) 0.051(2) -0.004(2) 0.0115(17) -0.011(2) C31 0.069(4) 0.059(4) 0.091(5) 0.006(3) 0.006(3) 0.002(3) C32 0.091(5) 0.088(5) 0.092(5) 0.031(4) -0.017(4) -0.010(4) C33 0.115(7) 0.131(8) 0.127(8) 0.069(6) -0.022(6) -0.037(6) C34 0.174(11) 0.121(8) 0.161(11) 0.067(8) -0.013(8) -0.028(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd O5 2.444(4) . ? Nd O5 2.444(4) 2 ? Nd O1 2.456(4) . ? Nd O1 2.456(4) 2 ? Nd O31 2.560(6) . ? Nd O31 2.560(6) 2 ? Nd O41 2.581(5) . ? Nd O41 2.581(5) 2 ? Nd O42 2.606(5) . ? Nd O42 2.606(5) 2 ? O1 C2 1.227(6) . ? C2 N21 1.358(7) . ? C2 C3 1.518(7) . ? C3 C4 1.517(7) . ? C3 C31 1.552(8) . ? C4 O5 1.250(6) . ? C4 N11 1.336(6) . ? N11 C13 1.440(6) . ? N11 C12 1.474(8) . ? C13 C18 1.376(8) . ? C13 C14 1.380(8) . ? C14 C15 1.397(10) . ? C15 C16 1.352(11) . ? C16 C17 1.383(11) . ? C17 C18 1.379(9) . ? N21 C23 1.435(7) . ? N21 C22 1.477(8) . ? C23 C24 1.368(8) . ? C23 C28 1.380(9) . ? C24 C25 1.401(11) . ? C25 C26 1.373(13) . ? C26 C27 1.356(13) . ? C27 C28 1.364(11) . ? N33 O34 1.234(11) . ? N33 O31 1.248(6) 2 ? N33 O31 1.249(6) . ? N43 O42 1.220(7) . ? N43 O44 1.243(6) . ? N43 O41 1.260(6) . ? C31 C32 1.515(10) . ? C32 C33 1.523(11) . ? C33 C34 1.409(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Nd O5 148.03(18) . 2 ? O5 Nd O1 69.74(13) . . ? O5 Nd O1 84.44(13) . 2 ? O1 Nd O1 72.4(3) . 2 ? O5 Nd O31 129.82(15) . . ? O1 Nd O31 137.12(19) . . ? O5 Nd O31 81.88(16) . 2 ? O1 Nd O31 137.20(17) . 2 ? O31 Nd O31 49.3(3) . 2 ? O5 Nd O41 117.61(12) . . ? O1 Nd O41 141.21(17) . . ? O31 Nd O41 70.37(17) . . ? O5 Nd O41 71.99(13) . 2 ? O1 Nd O41 70.91(18) . 2 ? O31 Nd O41 80.02(18) . 2 ? O41 Nd O41 147.5(2) . 2 ? O5 Nd O42 69.11(14) . . ? O1 Nd O42 124.41(17) . . ? O31 Nd O42 98.14(18) . . ? O41 Nd O42 48.62(14) . . ? O5 Nd O42 114.92(14) . 2 ? O1 Nd O42 68.04(18) . 2 ? O31 Nd O42 69.10(19) . 2 ? O41 Nd O42 126.51(14) . 2 ? O42 Nd O42 166.4(3) . 2 ? C2 O1 Nd 139.5(3) . . ? O1 C2 N21 118.5(5) . . ? O1 C2 C3 123.1(5) . . ? N21 C2 C3 118.4(5) . . ? C4 C3 C2 109.9(4) . . ? C4 C3 C31 109.5(4) . . ? C2 C3 C31 107.9(5) . . ? O5 C4 N11 120.5(5) . . ? O5 C4 C3 119.7(4) . . ? N11 C4 C3 119.7(4) . . ? C4 O5 Nd 126.4(3) . . ? C4 N11 C13 124.8(4) . . ? C4 N11 C12 118.5(4) . . ? C13 N11 C12 116.4(4) . . ? C18 C13 C14 121.5(5) . . ? C18 C13 N11 119.5(5) . . ? C14 C13 N11 118.9(5) . . ? C13 C14 C15 117.5(6) . . ? C16 C15 C14 121.4(7) . . ? C15 C16 C17 120.5(7) . . ? C18 C17 C16 119.3(6) . . ? C13 C18 C17 119.7(6) . . ? C2 N21 C23 124.4(5) . . ? C2 N21 C22 118.4(5) . . ? C23 N21 C22 117.0(5) . . ? C24 C23 C28 119.9(6) . . ? C24 C23 N21 120.8(6) . . ? C28 C23 N21 119.3(5) . . ? C23 C24 C25 119.2(7) . . ? C26 C25 C24 119.6(7) . . ? C27 C26 C25 120.6(8) . . ? C26 C27 C28 120.1(8) . . ? C27 C28 C23 120.6(7) . . ? O34 N33 O31 121.2(4) . 2 ? O34 N33 O31 121.3(4) . . ? O31 N33 O31 117.5(8) 2 . ? N33 O31 Nd 96.7(4) . . ? O42 N43 O44 121.6(6) . . ? O44 N43 O41 121.2(5) . . ? O42 N43 O41 117.2(5) . . ? N43 O41 Nd 97.4(3) . . ? N43 O44 Nd 96.7(3) . . ? C32 C31 C3 113.4(6) . . ? C31 C32 C33 111.7(7) . . ? C34 C33 C32 115.5(8) . . ? _refine_diff_density_max 1.238 _refine_diff_density_min -1.500 _refine_diff_density_rms 0.085 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Nd(L4)2(NO3)3 _chemical_formula_sum 'C42 H52 N7 Nd O15' _chemical_formula_weight 1039.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Nd' 'Nd' -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 27.76(3) _cell_length_b 18.22(2) _cell_length_c 19.12(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.730(10) _cell_angle_gamma 90.00 _cell_volume 9583(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4268 _exptl_absorpt_coefficient_mu 1.156 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.60 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number n/a _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33036 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.90 _reflns_number_total 17449 _reflns_number_gt 10787 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0933P)^2^+23.5002P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17449 _refine_ls_number_parameters 1183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1254 _refine_ls_R_factor_gt 0.0709 _refine_ls_wR_factor_ref 0.2022 _refine_ls_wR_factor_gt 0.1716 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.164 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.246484(13) 0.822126(19) 0.24846(2) 0.04027(13) Uani 1 d . . . O51A O 0.31990(18) 0.7807(3) 0.3384(3) 0.0568(13) Uani 1 d . . . N53A N 0.3459(2) 0.7599(3) 0.2937(4) 0.0551(16) Uani 1 d . . . O52A O 0.32593(19) 0.7576(3) 0.2287(3) 0.0585(14) Uani 1 d . . . O54A O 0.3886(2) 0.7418(4) 0.3086(4) 0.096(2) Uani 1 d . . . O61A O 0.2256(2) 0.7080(3) 0.1735(3) 0.0672(15) Uani 1 d . . . N63A N 0.2270(2) 0.6625(4) 0.2241(5) 0.064(2) Uani 1 d . . . O62A O 0.2371(2) 0.6893(3) 0.2855(4) 0.0720(17) Uani 1 d . . . O64A O 0.2183(3) 0.5970(4) 0.2128(5) 0.110(3) Uani 1 d . . . N73A N 0.1384(2) 0.8214(4) 0.1883(4) 0.0609(18) Uani 1 d . . . O71A O 0.1540(2) 0.7996(3) 0.2499(3) 0.0660(15) Uani 1 d . . . O72A O 0.17023(18) 0.8439(3) 0.1521(3) 0.0652(15) Uani 1 d . . . O74A O 0.0959(2) 0.8209(5) 0.1665(4) 0.122(3) Uani 1 d . . . O1A O 0.26673(15) 0.8667(3) 0.1362(2) 0.0430(11) Uani 1 d . . . C2A C 0.3084(2) 0.8813(3) 0.1229(3) 0.0350(14) Uani 1 d . . . C3A C 0.3339(2) 0.9522(4) 0.1528(4) 0.0416(15) Uani 1 d . . . H3A H 0.3656 0.9574 0.1360 0.050 Uiso 1 calc R . . C4A C 0.3404(2) 0.9501(3) 0.2333(4) 0.0396(15) Uani 1 d . . . O5A O 0.31410(18) 0.9132(3) 0.2661(3) 0.0514(12) Uani 1 d . . . C31A C 0.3006(3) 1.0178(4) 0.1268(5) 0.058(2) Uani 1 d . . . H31A H 0.2676 1.0072 0.1352 0.069 Uiso 1 calc R . . H31B H 0.3114 1.0613 0.1536 0.069 Uiso 1 calc R . . C32A C 0.3010(3) 1.0324(5) 0.0505(5) 0.068(2) Uani 1 d . . . H32A H 0.2919 0.9884 0.0233 0.081 Uiso 1 calc R . . H32B H 0.2779 1.0708 0.0347 0.081 Uiso 1 calc R . . O33A O 0.3481(2) 1.0540(3) 0.0411(3) 0.0731(18) Uani 1 d . . . C34A C 0.3555(5) 1.0604(6) -0.0296(6) 0.091(3) Uani 1 d . . . H34A H 0.3355 1.0998 -0.0519 0.109 Uiso 1 calc R . . H34B H 0.3460 1.0152 -0.0544 0.109 Uiso 1 calc R . . C35A C 0.4066(5) 1.0757(7) -0.0337(7) 0.120(5) Uani 1 d . . . H35A H 0.4155 1.1216 -0.0108 0.144 Uiso 1 calc R . . H35B H 0.4117 1.0785 -0.0823 0.144 Uiso 1 calc R . . H35C C 0.4263 1.0371 -0.0107 0.144 Uiso 1 calc R . . N21A N 0.3756(2) 0.9924(3) 0.2684(3) 0.0521(15) Uani 1 d . . . C22A C 0.3791(4) 0.9951(5) 0.3463(5) 0.082(3) Uani 1 d . . . H22A H 0.4122 1.0046 0.3661 0.099 Uiso 1 calc R . . H22B H 0.3689 0.9490 0.3636 0.099 Uiso 1 calc R . . H22C H 0.3586 1.0335 0.3598 0.099 Uiso 1 calc R . . C23A C 0.4077(2) 1.0398(4) 0.2362(4) 0.0470(17) Uani 1 d . . . C24A C 0.4454(3) 1.0113(5) 0.2061(5) 0.067(2) Uani 1 d . . . H24A H 0.4497 0.9607 0.2052 0.081 Uiso 1 calc R . . C25A C 0.4776(3) 1.0569(6) 0.1766(6) 0.085(3) Uani 1 d . . . H25A H 0.5024 1.0374 0.1541 0.102 Uiso 1 calc R . . C26A C 0.4718(4) 1.1313(6) 0.1816(6) 0.093(3) Uani 1 d . . . H26A H 0.4931 1.1627 0.1626 0.112 Uiso 1 calc R . . C27A C 0.4349(4) 1.1602(5) 0.2142(6) 0.082(3) Uani 1 d . . . H27A H 0.4320 1.2108 0.2186 0.098 Uiso 1 calc R . . C28A C 0.4023(3) 1.1143(4) 0.2406(5) 0.063(2) Uani 1 d . . . H28A H 0.3767 1.1338 0.2612 0.075 Uiso 1 calc R . . N11A N 0.33167(18) 0.8373(3) 0.0828(3) 0.0398(13) Uani 1 d . . . C12A C 0.3063(3) 0.7708(5) 0.0525(5) 0.084(3) Uani 1 d . . . H12A H 0.3192 0.7284 0.0783 0.101 Uiso 1 calc R . . H12B H 0.3112 0.7660 0.0039 0.101 Uiso 1 calc R . . H12C H 0.2722 0.7749 0.0555 0.101 Uiso 1 calc R . . C13A C 0.3814(3) 0.8436(4) 0.0708(4) 0.070(2) Uani 1 d . . . C14A C 0.3935(3) 0.8625(5) 0.0053(5) 0.076(3) Uani 1 d . . . H14A H 0.3694 0.8765 -0.0308 0.091 Uiso 1 calc R . . C15A C 0.4406(4) 0.8605(7) -0.0061(6) 0.107(4) Uani 1 d . . . H15A H 0.4489 0.8725 -0.0502 0.128 Uiso 1 calc R . . C16A C 0.4764(4) 0.8404(8) 0.0481(8) 0.114(5) Uani 1 d . . . H16A H 0.5087 0.8400 0.0403 0.137 Uiso 1 calc R . . C17A C 0.4650(3) 0.8214(5) 0.1121(7) 0.084(3) Uani 1 d . . . H17A H 0.4896 0.8070 0.1473 0.101 Uiso 1 calc R . . C18A C 0.4180(3) 0.8230(4) 0.1260(5) 0.061(2) Uani 1 d . . . H18A H 0.4104 0.8109 0.1705 0.073 Uiso 1 calc R . . O1B O 0.2125(2) 0.9436(3) 0.2675(3) 0.0573(14) Uani 1 d . . . C2B C 0.1771(3) 0.9621(4) 0.2960(4) 0.0503(19) Uani 1 d . . . C3B C 0.1763(3) 0.9445(4) 0.3742(4) 0.0465(17) Uani 1 d . . . H3B H 0.1448 0.9576 0.3887 0.056 Uiso 1 calc R . . C4B C 0.1866(2) 0.8623(4) 0.3852(4) 0.0470(17) Uani 1 d . . . O5B O 0.22441(17) 0.8343(3) 0.3684(3) 0.0509(12) Uani 1 d . . . C31B C 0.2184(3) 0.9867(4) 0.4190(5) 0.062(2) Uani 1 d . . . H31C H 0.2210 0.9701 0.4675 0.074 Uiso 1 calc R . . H31D H 0.2488 0.9750 0.4015 0.074 Uiso 1 calc R . . C32B C 0.2113(3) 1.0684(4) 0.4169(6) 0.073(3) Uani 1 d . . . H32C H 0.2379 1.0917 0.4470 0.087 Uiso 1 calc R . . H32D H 0.2119 1.0858 0.3691 0.087 Uiso 1 calc R . . O33B O 0.1658(2) 1.0893(3) 0.4401(3) 0.0704(17) Uani 1 d . . . C34B C 0.1640(4) 1.0921(5) 0.5123(6) 0.084(3) Uani 1 d . . . H34C H 0.1890 1.1247 0.5348 0.101 Uiso 1 calc R . . H34D H 0.1695 1.0436 0.5327 0.101 Uiso 1 calc R . . C35B C 0.1143(5) 1.1198(6) 0.5236(6) 0.116(5) Uani 1 d . . . H35D H 0.1111 1.1175 0.5730 0.140 Uiso 1 calc R . . H35E H 0.0897 1.0898 0.4975 0.140 Uiso 1 calc R . . H35F H 0.1105 1.1697 0.5076 0.140 Uiso 1 calc R . . N11B N 0.1422(2) 1.0031(4) 0.2620(4) 0.066(2) Uani 1 d . . . C12B C 0.1488(5) 1.0299(6) 0.1892(6) 0.114(5) Uani 1 d . . . H12D H 0.1410 1.0812 0.1853 0.137 Uiso 1 calc R . . H12E H 0.1277 1.0030 0.1545 0.137 Uiso 1 calc R . . H12F H 0.1820 1.0227 0.1816 0.137 Uiso 1 calc R . . C13B C 0.0968(3) 1.0230(5) 0.2861(5) 0.064(2) Uani 1 d . . . C14B C 0.0881(4) 1.0933(5) 0.3059(5) 0.080(3) Uani 1 d . . . H14B H 0.1120 1.1290 0.3058 0.095 Uiso 1 calc R . . C15B C 0.0439(5) 1.1110(8) 0.3259(7) 0.110(4) Uani 1 d . . . H15B H 0.0384 1.1583 0.3415 0.132 Uiso 1 calc R . . C16B C 0.0074(5) 1.0592(9) 0.3230(6) 0.114(5) Uani 1 d . . . H16B H -0.0230 1.0722 0.3343 0.137 Uiso 1 calc R . . C17B C 0.0163(4) 0.9875(7) 0.3031(7) 0.104(4) Uani 1 d . . . H17B H -0.0079 0.9520 0.3015 0.125 Uiso 1 calc R . . C18B C 0.0613(3) 0.9702(6) 0.2860(5) 0.080(3) Uani 1 d . . . H18B H 0.0679 0.9222 0.2740 0.096 Uiso 1 calc R . . N21B N 0.1556(2) 0.8217(3) 0.4174(3) 0.0433(14) Uani 1 d . . . C22B C 0.1651(3) 0.7417(4) 0.4256(5) 0.069(2) Uani 1 d . . . H22D H 0.1704 0.7294 0.4749 0.083 Uiso 1 calc R . . H22E H 0.1934 0.7291 0.4044 0.083 Uiso 1 calc R . . H22F H 0.1376 0.7148 0.4029 0.083 Uiso 1 calc R . . C23B C 0.1126(3) 0.8485(4) 0.4430(4) 0.0504(18) Uani 1 d . . . C24B C 0.1168(3) 0.8948(4) 0.5024(4) 0.064(2) Uani 1 d . . . H24B H 0.1473 0.9082 0.5249 0.077 Uiso 1 calc R . . C25B C 0.0753(5) 0.9204(5) 0.5272(6) 0.088(3) Uani 1 d . . . H25B H 0.0779 0.9530 0.5649 0.106 Uiso 1 calc R . . C26B C 0.0316(4) 0.8981(7) 0.4971(7) 0.100(4) Uani 1 d . . . H26B H 0.0040 0.9148 0.5148 0.120 Uiso 1 calc R . . C27B C 0.0262(4) 0.8504(8) 0.4396(7) 0.106(4) Uani 1 d . . . H27B H -0.0043 0.8345 0.4193 0.127 Uiso 1 calc R . . C28B C 0.0679(4) 0.8273(6) 0.4139(7) 0.096(4) Uani 1 d . . . H28B H 0.0649 0.7961 0.3751 0.115 Uiso 1 calc R . . Nd2 Nd 0.245731(13) 0.935744(19) 0.74875(2) 0.04071(13) Uani 1 d . . . N53C N 0.3536(2) 0.9325(4) 0.8033(5) 0.0642(19) Uani 1 d . . . O51C O 0.33816(18) 0.9558(3) 0.7455(3) 0.0628(14) Uani 1 d . . . O52C O 0.32232(18) 0.9096(3) 0.8430(3) 0.0602(14) Uani 1 d . . . O54C O 0.3972(2) 0.9285(5) 0.8269(4) 0.108(3) Uani 1 d . . . O51C O 0.3376(2) 0.9565(3) 0.7443(3) 0.0628(14) Uani 1 d . . . O62C O 0.17405(19) 0.9820(3) 0.6590(3) 0.0592(14) Uani 1 d . . . N63C N 0.1470(2) 1.0031(4) 0.7021(4) 0.0627(18) Uani 1 d . . . O61C O 0.16605(19) 1.0007(3) 0.7671(3) 0.0625(15) Uani 1 d . . . O64C O 0.1058(2) 1.0243(5) 0.6858(4) 0.100(2) Uani 1 d . . . O71C O 0.2688(2) 1.0474(3) 0.8261(3) 0.0633(14) Uani 1 d . . . O72C O 0.2854(3) 1.1552(3) 0.7916(4) 0.098(2) Uani 1 d . . . N73C N 0.2720(3) 1.0925(4) 0.7776(4) 0.0602(18) Uani 1 d . . . O74C O 0.2595(2) 1.0701(3) 0.7156(3) 0.0650(16) Uani 1 d . . . O1C O 0.17763(18) 0.8465(3) 0.7277(3) 0.0516(12) Uani 1 d . . . C2C C 0.1507(2) 0.8070(4) 0.7606(4) 0.0423(16) Uani 1 d . . . C3C C 0.1582(2) 0.8035(4) 0.8411(4) 0.0425(16) Uani 1 d . . . H3C H 0.1267 0.7960 0.8578 0.051 Uiso 1 calc R . . C4C C 0.1804(2) 0.8752(4) 0.8715(4) 0.0411(16) Uani 1 d . . . O5C O 0.22284(16) 0.8909(3) 0.8602(3) 0.0501(12) Uani 1 d . . . C31C C 0.1920(3) 0.7381(4) 0.8649(4) 0.0516(18) Uani 1 d . . . H31E H 0.1806 0.6947 0.8383 0.062 Uiso 1 calc R . . H31F H 0.2246 0.7489 0.8548 0.062 Uiso 1 calc R . . C32C C 0.1934(3) 0.7232(4) 0.9417(4) 0.062(2) Uani 1 d . . . H32E H 0.2176 0.6859 0.9566 0.074 Uiso 1 calc R . . H32F H 0.2021 0.7675 0.9686 0.074 Uiso 1 calc R . . O33C O 0.1470(2) 0.6988(3) 0.9535(3) 0.0610(14) Uani 1 d . . . C34C C 0.1421(5) 0.6901(6) 1.0259(5) 0.089(3) Uani 1 d . . . H34E H 0.1500 0.7358 1.0508 0.107 Uiso 1 calc R . . H34F H 0.1645 0.6527 1.0466 0.107 Uiso 1 calc R . . C35C C 0.0913(5) 0.6683(7) 1.0328(7) 0.113(4) Uani 1 d . . . H35G H 0.0887 0.6579 1.0813 0.136 Uiso 1 calc R . . H35H H 0.0828 0.6253 1.0047 0.136 Uiso 1 calc R . . H35I H 0.0696 0.7076 1.0166 0.136 Uiso 1 calc R . . N11C N 0.1168(2) 0.7651(3) 0.7239(3) 0.0509(15) Uani 1 d . . . C12C C 0.1138(3) 0.7628(5) 0.6470(4) 0.075(3) Uani 1 d . . . H12G H 0.1213 0.8104 0.6297 0.090 Uiso 1 calc R . . H12H H 0.0815 0.7490 0.6269 0.090 Uiso 1 calc R . . H12I H 0.1366 0.7275 0.6338 0.090 Uiso 1 calc R . . C13C C 0.0843(3) 0.7180(4) 0.7560(4) 0.0479(18) Uani 1 d . . . C14C C 0.0459(3) 0.7454(5) 0.7834(5) 0.071(2) Uani 1 d . . . H14C H 0.0405 0.7958 0.7824 0.085 Uiso 1 calc R . . C15C C 0.0137(4) 0.6985(8) 0.8137(6) 0.095(4) Uani 1 d . . . H15C H -0.0120 0.7171 0.8349 0.114 Uiso 1 calc R . . C16C C 0.0220(5) 0.6235(8) 0.8104(6) 0.099(4) Uani 1 d . . . H16C H 0.0012 0.5915 0.8296 0.119 Uiso 1 calc R . . C17C C 0.0598(4) 0.5954(6) 0.7798(6) 0.089(3) Uani 1 d . . . H17C H 0.0641 0.5449 0.7773 0.107 Uiso 1 calc R . . C18C C 0.0916(3) 0.6422(4) 0.7529(5) 0.066(2) Uani 1 d . . . H18C H 0.1177 0.6236 0.7328 0.079 Uiso 1 calc R . . N21C N 0.1559(2) 0.9176(3) 0.9112(3) 0.0538(16) Uani 1 d . . . C22C C 0.1803(4) 0.9846(5) 0.9419(5) 0.087(3) Uani 1 d . . . H22G H 0.1832 0.9822 0.9925 0.105 Uiso 1 calc R . . H22H H 0.1615 1.0269 0.9255 0.105 Uiso 1 calc R . . H22I H 0.2121 0.9882 0.9277 0.105 Uiso 1 calc R . . C23C C 0.1074(3) 0.9077(4) 0.9206(4) 0.0517(18) Uani 1 d . . . C24C C 0.0709(3) 0.9282(5) 0.8668(5) 0.071(3) Uani 1 d . . . H24C H 0.0791 0.9448 0.8239 0.085 Uiso 1 calc R . . C25C C 0.0227(4) 0.9240(6) 0.8771(7) 0.100(4) Uani 1 d . . . H25C H -0.0017 0.9380 0.8413 0.120 Uiso 1 calc R . . C26C C 0.0110(4) 0.8995(9) 0.9396(9) 0.131(5) Uani 1 d . . . H26C H -0.0214 0.8959 0.9464 0.157 Uiso 1 calc R . . C27C C 0.0474(5) 0.8796(9) 0.9935(8) 0.138(6) Uani 1 d . . . H27C H 0.0392 0.8634 1.0365 0.166 Uiso 1 calc R . . C28C C 0.0952(4) 0.8837(6) 0.9833(6) 0.095(4) Uani 1 d . . . H28C H 0.1194 0.8700 1.0194 0.114 Uiso 1 calc R . . O1D O 0.2788(2) 0.8153(3) 0.7281(3) 0.0585(14) Uani 1 d . . . C2D C 0.3127(3) 0.7956(4) 0.6980(4) 0.0483(17) Uani 1 d . . . C3D C 0.3127(3) 0.8163(3) 0.6196(4) 0.0465(18) Uani 1 d . . . H3D H 0.3441 0.8036 0.6048 0.056 Uiso 1 calc R . . C4D C 0.3035(3) 0.8985(4) 0.6098(4) 0.0454(17) Uani 1 d . . . N21D N 0.3331(2) 0.9404(3) 0.5774(3) 0.0478(15) Uani 1 d . . . O5D O 0.26522(18) 0.9253(3) 0.6278(3) 0.0505(12) Uani 1 d . . . C31D C 0.2714(3) 0.7752(4) 0.5731(4) 0.056(2) Uani 1 d . . . H31G H 0.2407 0.7862 0.5897 0.068 Uiso 1 calc R . . H31H H 0.2695 0.7928 0.5249 0.068 Uiso 1 calc R . . C32D C 0.2789(3) 0.6937(5) 0.5739(5) 0.070(3) Uani 1 d . . . H32G H 0.2767 0.6756 0.6210 0.084 Uiso 1 calc R . . H32H H 0.2528 0.6712 0.5421 0.084 Uiso 1 calc R . . O33D O 0.3239(3) 0.6713(3) 0.5539(4) 0.083(2) Uani 1 d . . . C34D C 0.3271(4) 0.6714(6) 0.4818(6) 0.089(3) Uani 1 d . . . H34G H 0.3193 0.7198 0.4623 0.107 Uiso 1 calc R . . H34H H 0.3040 0.6367 0.4579 0.107 Uiso 1 calc R . . C35D C 0.3782(5) 0.6504(7) 0.4703(7) 0.115(4) Uani 1 d . . . H35J H 0.3817 0.6562 0.4214 0.137 Uiso 1 calc R . . H35K H 0.3841 0.6001 0.4840 0.137 Uiso 1 calc R . . H35L H 0.4011 0.6814 0.4984 0.137 Uiso 1 calc R . . C22D C 0.3239(4) 1.0200(4) 0.5725(5) 0.073(3) Uani 1 d . . . H22J H 0.3259 1.0363 0.5253 0.088 Uiso 1 calc R . . H22K H 0.3477 1.0453 0.6049 0.088 Uiso 1 calc R . . H22L H 0.2920 1.0301 0.5843 0.088 Uiso 1 calc R . . C23D C 0.3763(3) 0.9157(4) 0.5518(5) 0.058(2) Uani 1 d . . . C24D C 0.3734(3) 0.8702(4) 0.4925(4) 0.058(2) Uani 1 d . . . H24D H 0.3430 0.8551 0.4708 0.070 Uiso 1 calc R . . C25D C 0.4145(4) 0.8471(6) 0.4656(6) 0.085(3) Uani 1 d . . . H25D H 0.4119 0.8148 0.4275 0.101 Uiso 1 calc R . . C26D C 0.4583(5) 0.8717(8) 0.4950(8) 0.118(5) Uani 1 d . . . H26D H 0.4861 0.8559 0.4772 0.142 Uiso 1 calc R . . C27D C 0.4625(5) 0.9190(9) 0.5500(9) 0.133(6) Uani 1 d . . . H27D H 0.4928 0.9376 0.5680 0.160 Uiso 1 calc R . . C28D C 0.4208(4) 0.9401(7) 0.5800(8) 0.119(5) Uani 1 d . . . H28D H 0.4239 0.9708 0.6192 0.143 Uiso 1 calc R . . N11D N 0.3480(2) 0.7537(3) 0.7288(4) 0.0600(18) Uani 1 d . . . C13D C 0.3917(3) 0.7319(5) 0.7018(5) 0.070(2) Uani 1 d . . . C12D C 0.3431(4) 0.7256(6) 0.8005(5) 0.101(4) Uani 1 d . . . H12J H 0.3569 0.6773 0.8061 0.121 Uiso 1 calc R . . H12K H 0.3093 0.7235 0.8064 0.121 Uiso 1 calc R . . H12L H 0.3599 0.7577 0.8354 0.121 Uiso 1 calc R . . C14D C 0.3988(4) 0.6598(6) 0.6871(6) 0.090(3) Uani 1 d . . . H14D H 0.3750 0.6249 0.6920 0.108 Uiso 1 calc R . . C15D C 0.4425(7) 0.6399(10) 0.6644(8) 0.147(7) Uani 1 d . . . H15D H 0.4481 0.5909 0.6542 0.177 Uiso 1 calc R . . C16D C 0.4776(6) 0.6914(15) 0.6569(11) 0.176(12) Uani 1 d . . . H16D H 0.5071 0.6770 0.6431 0.211 Uiso 1 calc R . . C17D C 0.4692(5) 0.7635(12) 0.6696(8) 0.150(7) Uani 1 d . . . H17D H 0.4921 0.7989 0.6619 0.181 Uiso 1 calc R . . C18D C 0.4260(4) 0.7840(7) 0.6944(6) 0.102(4) Uani 1 d . . . H18D H 0.4207 0.8327 0.7057 0.122 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Nd1 0.0397(2) 0.0391(2) 0.0434(3) 0.00199(16) 0.01066(18) -0.00081(14) O51A 0.052(3) 0.072(4) 0.048(3) 0.012(3) 0.010(3) 0.008(3) N53A 0.045(4) 0.053(4) 0.066(5) 0.011(3) 0.005(3) 0.011(3) O52A 0.053(3) 0.068(4) 0.054(4) 0.000(3) 0.003(3) 0.011(2) O54A 0.057(4) 0.149(7) 0.078(5) -0.001(4) -0.005(3) 0.032(4) O61A 0.076(4) 0.052(4) 0.075(4) -0.010(3) 0.012(3) -0.009(3) N63A 0.062(4) 0.040(4) 0.097(7) -0.011(4) 0.036(4) -0.012(3) O62A 0.089(5) 0.054(4) 0.077(5) 0.000(3) 0.022(4) -0.003(3) O64A 0.133(7) 0.050(4) 0.157(8) -0.028(4) 0.060(6) -0.035(4) N73A 0.032(3) 0.088(5) 0.060(5) -0.006(4) -0.001(3) 0.002(3) O71A 0.052(3) 0.089(4) 0.058(4) 0.008(3) 0.011(3) -0.012(3) O72A 0.038(3) 0.100(4) 0.057(4) 0.008(3) 0.005(3) 0.001(3) O74A 0.043(4) 0.210(10) 0.106(7) 0.004(6) -0.010(4) -0.007(4) O1A 0.029(2) 0.062(3) 0.038(3) 0.004(2) 0.0037(19) -0.0031(19) C2A 0.032(3) 0.042(4) 0.030(4) 0.010(3) 0.000(3) 0.005(3) C3A 0.044(4) 0.037(4) 0.045(4) 0.001(3) 0.010(3) 0.001(3) C4A 0.040(4) 0.028(3) 0.052(5) -0.001(3) 0.009(3) 0.003(3) O5A 0.062(3) 0.046(3) 0.048(3) 0.002(2) 0.016(3) -0.005(2) C31A 0.048(4) 0.040(4) 0.085(7) 0.008(4) 0.007(4) 0.008(3) C32A 0.069(6) 0.053(5) 0.075(7) 0.022(4) -0.011(5) -0.001(4) O33A 0.086(4) 0.081(4) 0.049(4) 0.021(3) 0.000(3) -0.026(3) C34A 0.133(10) 0.077(7) 0.062(7) 0.015(5) 0.009(7) -0.013(6) C35A 0.126(11) 0.134(11) 0.108(11) 0.006(8) 0.041(9) -0.027(8) N21A 0.064(4) 0.049(4) 0.043(4) 0.002(3) 0.004(3) -0.014(3) C22A 0.098(7) 0.083(7) 0.064(7) -0.007(5) 0.004(5) -0.036(5) C23A 0.040(4) 0.048(4) 0.052(5) 0.010(3) 0.002(3) -0.010(3) C24A 0.057(5) 0.065(6) 0.077(7) -0.001(4) -0.004(4) -0.003(4) C25A 0.045(5) 0.105(9) 0.107(9) -0.002(6) 0.017(5) -0.011(5) C26A 0.095(8) 0.095(9) 0.094(9) 0.006(6) 0.030(7) -0.047(6) C27A 0.094(7) 0.054(6) 0.097(8) 0.014(5) 0.012(6) -0.022(5) C28A 0.058(5) 0.052(5) 0.078(6) 0.006(4) 0.008(4) -0.009(4) N11A 0.033(3) 0.045(3) 0.042(4) -0.010(3) 0.008(2) 0.000(2) C12A 0.076(6) 0.082(7) 0.096(8) -0.052(6) 0.017(5) -0.021(5) C13A 0.062(4) 0.058(4) 0.093(6) -0.007(4) 0.020(4) 0.006(3) C14A 0.081(6) 0.115(8) 0.037(5) 0.022(5) 0.027(4) 0.015(5) C15A 0.092(8) 0.163(12) 0.075(8) 0.026(8) 0.048(7) 0.025(8) C16A 0.074(8) 0.142(11) 0.141(13) 0.005(9) 0.067(9) -0.002(7) C17A 0.035(4) 0.103(8) 0.114(10) 0.003(6) 0.004(5) 0.019(4) C18A 0.052(5) 0.067(6) 0.059(6) 0.006(4) -0.004(4) 0.010(4) O1B 0.069(4) 0.044(3) 0.064(4) 0.016(2) 0.026(3) 0.005(2) C2B 0.052(4) 0.034(4) 0.071(6) 0.011(3) 0.028(4) 0.001(3) C3B 0.051(4) 0.035(4) 0.054(5) 0.000(3) 0.012(3) -0.003(3) C4B 0.037(4) 0.048(4) 0.055(5) -0.014(3) 0.003(3) -0.005(3) O5B 0.048(3) 0.059(3) 0.046(3) 0.000(2) 0.009(2) 0.010(2) C31B 0.051(5) 0.064(5) 0.069(6) -0.013(4) 0.002(4) 0.000(4) C32B 0.073(6) 0.060(6) 0.087(8) -0.011(4) 0.018(5) -0.006(4) O33B 0.088(4) 0.055(4) 0.066(4) -0.019(3) 0.004(3) 0.006(3) C34B 0.114(9) 0.063(6) 0.076(8) -0.012(5) 0.012(6) -0.012(5) C35B 0.168(13) 0.099(9) 0.099(10) -0.014(7) 0.080(9) -0.007(8) N11B 0.067(4) 0.056(4) 0.080(5) 0.025(4) 0.027(4) 0.018(3) C12B 0.150(11) 0.107(9) 0.096(9) 0.050(7) 0.059(8) 0.065(8) C13B 0.057(5) 0.077(6) 0.058(6) -0.003(4) 0.008(4) 0.017(4) C14B 0.079(6) 0.073(6) 0.083(7) 0.004(5) -0.002(5) 0.027(5) C15B 0.099(9) 0.124(11) 0.104(10) -0.029(8) 0.005(8) 0.060(8) C16B 0.088(9) 0.187(15) 0.069(8) 0.000(8) 0.013(7) 0.068(9) C17B 0.069(7) 0.129(10) 0.118(11) 0.001(8) 0.024(7) 0.004(7) C18B 0.070(6) 0.079(7) 0.089(8) 0.016(5) 0.006(5) 0.010(5) N21B 0.046(3) 0.044(4) 0.042(4) 0.004(2) 0.009(3) -0.002(2) C22B 0.082(6) 0.046(5) 0.082(7) 0.016(4) 0.023(5) 0.005(4) C23B 0.062(5) 0.045(4) 0.050(5) 0.002(3) 0.024(4) -0.004(3) C24B 0.091(6) 0.065(5) 0.041(5) -0.006(4) 0.026(4) -0.020(4) C25B 0.126(10) 0.065(6) 0.087(8) -0.008(5) 0.061(7) -0.002(6) C26B 0.083(8) 0.098(9) 0.128(11) 0.001(7) 0.050(8) -0.005(6) C27B 0.066(7) 0.136(10) 0.118(11) -0.036(9) 0.019(7) -0.027(7) C28B 0.062(6) 0.104(8) 0.121(10) -0.045(7) 0.011(6) -0.023(5) Nd2 0.0404(2) 0.0392(2) 0.0436(3) -0.00177(16) 0.00979(18) -0.00327(14) N53C 0.031(3) 0.086(5) 0.072(5) -0.010(4) -0.002(3) 0.000(3) O52C 0.041(3) 0.077(4) 0.062(4) -0.001(3) 0.004(3) 0.000(3) O54C 0.036(3) 0.191(8) 0.093(6) 0.006(5) -0.008(3) -0.010(4) O51C 0.049(3) 0.088(4) 0.050(3) -0.002(3) 0.004(3) -0.013(3) O62C 0.052(3) 0.075(4) 0.051(3) 0.009(3) 0.009(3) 0.010(3) N63C 0.043(4) 0.076(5) 0.068(5) 0.011(4) 0.001(3) 0.011(3) O61C 0.058(3) 0.075(4) 0.055(4) 0.005(3) 0.007(3) 0.022(3) O64C 0.056(4) 0.155(7) 0.084(5) -0.006(5) -0.009(3) 0.039(4) O71C 0.075(4) 0.053(3) 0.060(4) -0.012(3) 0.002(3) -0.005(3) O72C 0.129(6) 0.049(4) 0.120(6) -0.023(4) 0.032(5) -0.023(4) N73C 0.075(5) 0.038(4) 0.072(5) -0.012(4) 0.029(4) -0.006(3) O74C 0.094(5) 0.044(3) 0.059(4) -0.003(3) 0.018(3) -0.007(3) O1C 0.058(3) 0.054(3) 0.044(3) -0.004(2) 0.013(2) -0.015(2) C2C 0.039(4) 0.048(4) 0.040(4) -0.004(3) 0.008(3) -0.001(3) C3C 0.036(3) 0.043(4) 0.049(5) 0.006(3) 0.006(3) 0.002(3) C4C 0.031(3) 0.048(4) 0.044(4) 0.007(3) 0.007(3) -0.004(3) O5C 0.040(3) 0.055(3) 0.055(3) -0.003(2) 0.006(2) -0.010(2) C31C 0.045(4) 0.049(4) 0.059(5) 0.004(3) 0.002(4) 0.004(3) C32C 0.067(5) 0.045(5) 0.066(6) 0.016(4) -0.022(4) -0.005(4) O33C 0.066(4) 0.072(4) 0.042(3) 0.012(3) -0.002(3) -0.015(3) C34C 0.129(10) 0.082(8) 0.054(7) 0.016(5) 0.002(6) -0.005(6) C35C 0.123(11) 0.116(10) 0.110(11) 0.030(8) 0.046(8) 0.001(8) N11C 0.055(4) 0.047(4) 0.048(4) 0.006(3) 0.001(3) -0.012(3) C12C 0.086(7) 0.078(6) 0.058(6) -0.002(4) 0.000(5) -0.030(5) C13C 0.051(4) 0.053(5) 0.038(4) 0.006(3) -0.001(3) -0.018(3) C14C 0.052(5) 0.083(6) 0.078(7) -0.005(5) 0.007(5) -0.013(4) C15C 0.053(6) 0.151(11) 0.084(8) -0.025(7) 0.021(5) -0.032(6) C16C 0.099(9) 0.123(11) 0.079(8) 0.005(7) 0.023(7) -0.056(8) C17C 0.112(9) 0.065(6) 0.085(8) 0.023(5) -0.011(7) -0.040(6) C18C 0.068(5) 0.057(5) 0.070(6) 0.012(4) -0.003(4) -0.016(4) N21C 0.056(4) 0.060(4) 0.046(4) -0.003(3) 0.010(3) -0.003(3) C22C 0.103(8) 0.074(7) 0.092(8) -0.043(6) 0.037(6) -0.025(5) C23C 0.050(4) 0.055(5) 0.052(5) -0.001(4) 0.015(4) 0.006(3) C24C 0.071(6) 0.081(6) 0.062(6) 0.009(4) 0.010(5) 0.015(4) C25C 0.048(6) 0.141(10) 0.112(10) 0.010(8) 0.011(6) 0.018(6) C26C 0.071(8) 0.175(13) 0.161(15) 0.027(11) 0.065(9) 0.017(8) C27C 0.114(10) 0.210(16) 0.106(11) 0.066(11) 0.074(9) 0.056(11) C28C 0.095(8) 0.122(9) 0.077(8) 0.033(6) 0.043(6) 0.021(6) O1D 0.072(4) 0.050(3) 0.060(4) 0.006(2) 0.031(3) 0.005(2) C2D 0.059(5) 0.032(4) 0.055(5) -0.002(3) 0.009(4) -0.004(3) C3D 0.051(4) 0.034(4) 0.056(5) -0.007(3) 0.011(4) 0.004(3) C4D 0.048(4) 0.048(4) 0.040(4) -0.008(3) 0.004(3) -0.004(3) N21D 0.059(4) 0.042(4) 0.044(4) -0.001(3) 0.011(3) -0.003(3) O5D 0.052(3) 0.063(3) 0.037(3) 0.001(2) 0.011(2) 0.010(2) C31D 0.053(4) 0.047(5) 0.069(6) -0.011(4) 0.005(4) -0.006(3) C32D 0.081(6) 0.066(6) 0.066(6) -0.023(4) 0.017(5) -0.018(4) O33D 0.116(6) 0.070(4) 0.065(5) -0.013(3) 0.022(4) 0.026(4) C34D 0.111(9) 0.081(7) 0.081(8) -0.009(5) 0.027(7) -0.018(6) C35D 0.163(13) 0.096(9) 0.098(10) -0.007(7) 0.069(9) 0.009(8) C22D 0.105(7) 0.050(5) 0.070(6) 0.006(4) 0.037(5) -0.007(4) C23D 0.047(4) 0.049(5) 0.080(6) 0.001(4) 0.017(4) -0.013(3) C24D 0.070(5) 0.053(5) 0.054(5) 0.001(4) 0.018(4) -0.003(4) C25D 0.107(8) 0.085(7) 0.068(7) 0.009(5) 0.033(6) 0.009(6) C26D 0.090(9) 0.158(13) 0.116(11) -0.020(9) 0.052(8) -0.023(8) C27D 0.068(8) 0.189(15) 0.142(14) -0.034(11) 0.014(8) -0.037(8) C28D 0.066(7) 0.158(12) 0.134(12) -0.065(9) 0.015(7) -0.032(7) N11D 0.066(4) 0.052(4) 0.064(5) 0.008(3) 0.018(4) 0.016(3) C13D 0.066(6) 0.086(7) 0.054(6) -0.003(4) -0.001(4) 0.019(5) C12D 0.122(9) 0.115(9) 0.069(7) 0.034(6) 0.024(6) 0.053(7) C14D 0.102(8) 0.074(7) 0.093(8) 0.006(6) 0.008(6) 0.035(6) C15D 0.165(15) 0.166(16) 0.107(12) -0.014(11) 0.008(12) 0.116(14) C16D 0.082(10) 0.32(3) 0.118(14) -0.033(17) 0.000(10) 0.098(15) C17D 0.054(7) 0.28(2) 0.114(12) -0.031(14) 0.009(7) -0.006(10) C18D 0.069(7) 0.133(10) 0.103(9) -0.028(7) 0.012(6) -0.017(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nd1 O1A 2.431(5) . ? Nd1 O1B 2.452(5) . ? Nd1 O5B 2.462(5) . ? Nd1 O5A 2.494(5) . ? Nd1 O62A 2.545(6) . ? Nd1 O61A 2.548(6) . ? Nd1 O52A 2.571(5) . ? Nd1 O51A 2.596(5) . ? Nd1 O71A 2.604(6) . ? Nd1 O72A 2.643(6) . ? O51A N53A 1.249(8) . ? N53A O54A 1.227(8) . ? N53A O52A 1.291(8) . ? O61A N63A 1.270(9) . ? N63A O64A 1.231(8) . ? N63A O62A 1.268(9) . ? N73A O74A 1.197(9) . ? N73A O72A 1.262(8) . ? N73A O71A 1.263(9) . ? O1A C2A 1.246(7) . ? C2A N11A 1.335(8) . ? C2A C3A 1.546(9) . ? C3A C4A 1.526(10) . ? C3A C31A 1.552(9) . ? C4A O5A 1.226(8) . ? C4A N21A 1.350(9) . ? C31A C32A 1.484(11) . ? C32A O33A 1.399(10) . ? O33A C34A 1.399(11) . ? C34A C35A 1.458(16) . ? N21A C23A 1.438(9) . ? N21A C22A 1.481(10) . ? C23A C24A 1.365(11) . ? C23A C28A 1.369(11) . ? C24A C25A 1.394(13) . ? C25A C26A 1.370(14) . ? C26A C27A 1.373(14) . ? C27A C28A 1.377(11) . ? N11A C13A 1.435(8) . ? N11A C12A 1.479(9) . ? C13A C14A 1.383(10) . ? C13A C18A 1.415(11) . ? C14A C15A 1.355(13) . ? C15A C16A 1.385(17) . ? C16A C17A 1.349(16) . ? C17A C18A 1.366(12) . ? O1B C2B 1.232(8) . ? C2B N11B 1.323(9) . ? C2B C3B 1.533(11) . ? C3B C4B 1.534(10) . ? C3B C31B 1.556(10) . ? C4B O5B 1.247(8) . ? C4B N21B 1.345(9) . ? C31B C32B 1.503(11) . ? C32B O33B 1.445(10) . ? O33B C34B 1.388(11) . ? C34B C35B 1.512(15) . ? N11B C13B 1.444(10) . ? N11B C12B 1.509(11) . ? C13B C14B 1.366(12) . ? C13B C18B 1.378(13) . ? C14B C15B 1.373(14) . ? C15B C16B 1.379(18) . ? C16B C17B 1.392(17) . ? C17B C18B 1.370(13) . ? N21B C23B 1.434(9) . ? N21B C22B 1.487(9) . ? C23B C28B 1.348(12) . ? C23B C24B 1.407(11) . ? C24B C25B 1.383(13) . ? C25B C26B 1.336(16) . ? C26B C27B 1.393(16) . ? C27B C28B 1.381(14) . ? Nd2 O1D 2.431(5) . ? Nd2 O5C 2.444(5) . ? Nd2 O5D 2.452(5) . ? Nd2 O1C 2.485(5) . ? Nd2 O71C 2.545(6) . ? Nd2 O72C 2.571(6) . ? Nd2 O61C 2.574(5) . ? Nd2 O62C 2.587(5) . ? Nd2 O51C 2.590(6) . ? Nd2 O52C 2.639(6) . ? O51C N53C 1.236(10) . ? N53C O54C 1.238(9) . ? N53C O52C 1.295(9) . ? O62C N63C 1.248(8) . ? N63C O64C 1.208(8) . ? N63C O61C 1.285(8) . ? O71C N73C 1.252(8) . ? O74C N73C 1.219(8) . ? N73C O72C 1.257(9) . ? O1C C2C 1.265(8) . ? C2C N11C 1.336(9) . ? C2C C3C 1.525(10) . ? C3C C4C 1.526(9) . ? C3C C31C 1.547(9) . ? C4C O5C 1.258(7) . ? C4C N21C 1.331(9) . ? C31C C32C 1.489(11) . ? C32C O33C 1.410(10) . ? O33C C34C 1.416(11) . ? C34C C35C 1.489(15) . ? N11C C13C 1.443(8) . ? N11C C12C 1.463(10) . ? C13C C14C 1.343(11) . ? C13C C18C 1.398(11) . ? C14C C15C 1.417(13) . ? C15C C16C 1.388(16) . ? C16C C17C 1.368(16) . ? C17C C18C 1.375(12) . ? N21C C23C 1.396(9) . ? N21C C22C 1.479(10) . ? C23C C28C 1.362(12) . ? C23C C24C 1.393(12) . ? C24C C25C 1.382(13) . ? C25C C26C 1.355(17) . ? C26C C27C 1.391(19) . ? C27C C28C 1.368(15) . ? O1D C2D 1.222(8) . ? C2D N11D 1.316(9) . ? C2D C3D 1.546(11) . ? C3D C4D 1.527(9) . ? C3D C31D 1.547(10) . ? C4D O5D 1.258(8) . ? C4D N21D 1.336(9) . ? N21D C23D 1.425(10) . ? N21D C22D 1.474(10) . ? C31D C32D 1.500(11) . ? C32D O33D 1.415(11) . ? O33D C34D 1.394(12) . ? C34D C35D 1.512(15) . ? C23D C28D 1.356(13) . ? C23D C24D 1.398(11) . ? C24D C25D 1.379(12) . ? C25D C26D 1.346(16) . ? C26D C27D 1.354(17) . ? C27D C28D 1.412(17) . ? N11D C13D 1.435(11) . ? N11D C12D 1.489(11) . ? C13D C14D 1.363(13) . ? C13D C18D 1.367(14) . ? C14D C15D 1.390(18) . ? C15D C16D 1.37(3) . ? C16D C17D 1.36(3) . ? C17D C18D 1.398(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Nd1 O1B 88.20(17) . . ? O1A Nd1 O5B 155.31(17) . . ? O1B Nd1 O5B 68.39(17) . . ? O1A Nd1 O5A 68.79(16) . . ? O1B Nd1 O5A 71.15(19) . . ? O5B Nd1 O5A 95.21(17) . . ? O1A Nd1 O62A 127.44(19) . . ? O1B Nd1 O62A 139.57(19) . . ? O5B Nd1 O62A 77.23(19) . . ? O5A Nd1 O62A 134.3(2) . . ? O1A Nd1 O61A 80.68(19) . . ? O1B Nd1 O61A 139.2(2) . . ? O5B Nd1 O61A 122.10(19) . . ? O5A Nd1 O61A 136.82(18) . . ? O62A Nd1 O61A 49.9(2) . . ? O1A Nd1 O52A 73.63(16) . . ? O1B Nd1 O52A 142.10(17) . . ? O5B Nd1 O52A 120.26(17) . . ? O5A Nd1 O52A 71.31(19) . . ? O62A Nd1 O52A 74.24(19) . . ? O61A Nd1 O52A 71.24(19) . . ? O1A Nd1 O51A 115.36(16) . . ? O1B Nd1 O51A 116.61(19) . . ? O5B Nd1 O51A 71.37(17) . . ? O5A Nd1 O51A 66.08(18) . . ? O62A Nd1 O51A 68.9(2) . . ? O61A Nd1 O51A 103.51(19) . . ? O52A Nd1 O51A 49.62(18) . . ? O1A Nd1 O71A 114.04(17) . . ? O1B Nd1 O71A 75.01(19) . . ? O5B Nd1 O71A 68.61(18) . . ? O5A Nd1 O71A 145.96(18) . . ? O62A Nd1 O71A 73.1(2) . . ? O61A Nd1 O71A 74.18(19) . . ? O52A Nd1 O71A 142.72(19) . . ? O51A Nd1 O71A 129.38(18) . . ? O1A Nd1 O72A 65.96(17) . . ? O1B Nd1 O72A 71.3(2) . . ? O5B Nd1 O72A 111.08(18) . . ? O5A Nd1 O72A 120.80(18) . . ? O62A Nd1 O72A 103.5(2) . . ? O61A Nd1 O72A 68.3(2) . . ? O52A Nd1 O72A 126.04(19) . . ? O51A Nd1 O72A 171.65(17) . . ? O71A Nd1 O72A 48.14(18) . . ? N53A O51A Nd1 96.2(4) . . ? O54A N53A O51A 123.4(7) . . ? O54A N53A O52A 119.4(7) . . ? O51A N53A O52A 117.2(6) . . ? N53A O52A Nd1 96.3(4) . . ? N63A O61A Nd1 97.1(5) . . ? O64A N63A O62A 123.4(8) . . ? O64A N63A O61A 121.0(9) . . ? O62A N63A O61A 115.7(7) . . ? N63A O62A Nd1 97.3(5) . . ? O74A N73A O72A 122.7(8) . . ? O74A N73A O71A 121.4(8) . . ? O72A N73A O71A 115.9(6) . . ? N73A O71A Nd1 98.9(4) . . ? N73A O72A Nd1 97.0(4) . . ? C2A O1A Nd1 125.7(4) . . ? O1A C2A N11A 121.5(6) . . ? O1A C2A C3A 119.7(6) . . ? N11A C2A C3A 118.8(5) . . ? C4A C3A C2A 109.8(5) . . ? C4A C3A C31A 109.1(6) . . ? C2A C3A C31A 107.5(6) . . ? O5A C4A N21A 120.0(7) . . ? O5A C4A C3A 122.2(6) . . ? N21A C4A C3A 117.8(6) . . ? C4A O5A Nd1 141.7(5) . . ? C32A C31A C3A 111.7(7) . . ? O33A C32A C31A 108.0(7) . . ? C34A O33A C32A 114.2(8) . . ? O33A C34A C35A 109.8(10) . . ? C4A N21A C23A 125.4(6) . . ? C4A N21A C22A 117.7(6) . . ? C23A N21A C22A 116.7(6) . . ? C24A C23A C28A 120.0(7) . . ? C24A C23A N21A 120.4(7) . . ? C28A C23A N21A 119.4(7) . . ? C23A C24A C25A 120.9(9) . . ? C26A C25A C24A 118.3(10) . . ? C25A C26A C27A 120.9(9) . . ? C28A C27A C26A 120.0(9) . . ? C23A C28A C27A 119.8(9) . . ? C2A N11A C13A 126.5(6) . . ? C2A N11A C12A 118.4(6) . . ? C13A N11A C12A 114.8(6) . . ? C14A C13A C18A 120.4(7) . . ? C14A C13A N11A 121.4(7) . . ? C18A C13A N11A 118.0(7) . . ? C15A C14A C13A 119.7(9) . . ? C14A C15A C16A 119.8(10) . . ? C17A C16A C15A 121.1(10) . . ? C16A C17A C18A 121.1(10) . . ? C17A C18A C13A 118.0(9) . . ? C2B O1B Nd1 131.2(4) . . ? O1B C2B N11B 120.8(7) . . ? O1B C2B C3B 119.5(7) . . ? N11B C2B C3B 119.4(6) . . ? C4B C3B C2B 108.1(6) . . ? C4B C3B C31B 107.0(6) . . ? C2B C3B C31B 108.9(6) . . ? O5B C4B N21B 120.3(7) . . ? O5B C4B C3B 120.9(6) . . ? N21B C4B C3B 118.7(6) . . ? C4B O5B Nd1 126.9(5) . . ? C32B C31B C3B 112.8(7) . . ? O33B C32B C31B 111.8(7) . . ? C34B O33B C32B 117.7(8) . . ? O33B C34B C35B 108.1(9) . . ? C2B N11B C13B 126.7(7) . . ? C2B N11B C12B 117.6(7) . . ? C13B N11B C12B 115.6(7) . . ? C14B C13B C18B 120.1(9) . . ? C14B C13B N11B 121.3(9) . . ? C18B C13B N11B 118.6(8) . . ? C13B C14B C15B 119.8(11) . . ? C14B C15B C16B 120.4(12) . . ? C15B C16B C17B 119.9(11) . . ? C18B C17B C16B 118.8(12) . . ? C17B C18B C13B 121.0(10) . . ? C4B N21B C23B 125.6(6) . . ? C4B N21B C22B 118.2(6) . . ? C23B N21B C22B 116.2(6) . . ? C28B C23B C24B 118.4(8) . . ? C28B C23B N21B 121.6(8) . . ? C24B C23B N21B 119.9(7) . . ? C25B C24B C23B 119.9(9) . . ? C26B C25B C24B 119.9(10) . . ? C25B C26B C27B 121.6(10) . . ? C28B C27B C26B 117.7(10) . . ? C23B C28B C27B 122.3(10) . . ? O1D Nd2 O5C 89.31(18) . . ? O1D Nd2 O5D 68.97(17) . . ? O5C Nd2 O5D 155.84(17) . . ? O1D Nd2 O1C 71.24(19) . . ? O5C Nd2 O1C 68.99(16) . . ? O5D Nd2 O1C 93.21(17) . . ? O1D Nd2 O71C 138.1(2) . . ? O5C Nd2 O71C 80.52(19) . . ? O5D Nd2 O71C 122.64(19) . . ? O1C Nd2 O71C 138.04(18) . . ? O1D Nd2 O72C 138.40(19) . . ? O5C Nd2 O72C 126.72(18) . . ? O5D Nd2 O72C 77.42(18) . . ? O1C Nd2 O72C 135.95(19) . . ? O71C Nd2 O72C 49.3(2) . . ? O1D Nd2 O61C 141.93(19) . . ? O5C Nd2 O61C 72.90(17) . . ? O5D Nd2 O61C 117.83(17) . . ? O1C Nd2 O61C 71.0(2) . . ? O71C Nd2 O61C 72.94(19) . . ? O72C Nd2 O61C 75.8(2) . . ? O1D Nd2 O62C 117.4(2) . . ? O5C Nd2 O62C 114.84(17) . . ? O5D Nd2 O62C 69.35(18) . . ? O1C Nd2 O62C 66.75(18) . . ? O71C Nd2 O62C 103.64(19) . . ? O72C Nd2 O62C 69.71(19) . . ? O61C Nd2 O62C 48.90(18) . . ? O1D Nd2 O51C 74.5(2) . . ? O5C Nd2 O51C 116.74(17) . . ? O5D Nd2 O51C 68.73(17) . . ? O1C Nd2 O51C 145.19(19) . . ? O71C Nd2 O51C 74.36(19) . . ? O72C Nd2 O51C 70.9(2) . . ? O61C Nd2 O51C 143.6(2) . . ? O62C Nd2 O51C 127.08(18) . . ? O1D Nd2 O52C 70.18(19) . . ? O5C Nd2 O52C 67.94(18) . . ? O5D Nd2 O52C 111.73(18) . . ? O1C Nd2 O52C 121.20(18) . . ? O71C Nd2 O52C 68.36(19) . . ? O72C Nd2 O52C 101.95(19) . . ? O61C Nd2 O52C 128.17(19) . . ? O62C Nd2 O52C 171.38(17) . . ? O51C Nd2 O52C 48.91(18) . . ? O51C N53C O54C 124.6(8) . . ? O51C N53C O52C 117.5(6) . . ? O54C N53C O52C 117.9(9) . . ? O51C O52C Nd2 94.8(5) . . ? O51C N53C Nd2 98.7(4) . . ? N63C O62C Nd2 98.0(4) . . ? O64C N63C O62C 124.1(8) . . ? O64C N63C O61C 120.9(7) . . ? O62C N63C O61C 115.0(6) . . ? N63C O61C Nd2 97.6(4) . . ? N73C O71C Nd2 97.6(5) . . ? O74C N73C O71C 120.2(8) . . ? O74C N73C O74C 123.2(8) . . ? O71C N73C O72C 116.5(6) . . ? N73C O72C Nd2 96.2(4) . . ? C2C O1C Nd2 141.2(5) . . ? O1C C2C N11C 119.0(7) . . ? O1C C2C C3C 121.1(6) . . ? N11C C2C C3C 119.8(6) . . ? C4C C3C C2C 110.0(5) . . ? C4C C3C C31C 110.4(6) . . ? C2C C3C C31C 108.9(6) . . ? O5C C4C N21C 121.8(6) . . ? O5C C4C C3C 118.0(6) . . ? N21C C4C C3C 120.2(6) . . ? C4C O5C Nd2 125.8(4) . . ? C32C C31C C3C 111.4(6) . . ? O33C C32C C31C 108.2(6) . . ? C32C O33C C34C 113.6(7) . . ? O33C C34C C35C 109.4(9) . . ? C2C N11C C13C 123.6(6) . . ? C2C N11C C12C 119.1(6) . . ? C13C N11C C12C 117.2(6) . . ? C14C C13C C18C 120.8(7) . . ? C14C C13C N11C 121.2(8) . . ? C18C C13C N11C 117.8(7) . . ? C13C C14C C15C 120.7(10) . . ? C16C C15C C14C 117.2(10) . . ? C17C C16C C15C 122.0(9) . . ? C16C C17C C18C 119.6(11) . . ? C17C C18C C13C 119.5(9) . . ? C4C N21C C23C 125.1(6) . . ? C4C N21C C22C 117.6(6) . . ? C23C N21C C22C 117.0(7) . . ? C28C C23C N21C 120.9(8) . . ? C28C C23C C24C 119.7(8) . . ? N21C C23C C24C 119.2(7) . . ? C25C C24C C23C 120.1(10) . . ? C26C C25C C24C 119.6(11) . . ? C25C C26C C27C 120.3(11) . . ? C28C C27C C26C 120.1(11) . . ? C27C C28C C23C 120.2(11) . . ? C2D O1D Nd2 132.4(5) . . ? O1D C2D N11D 122.4(8) . . ? O1D C2D C3D 119.0(7) . . ? N11D C2D C3D 118.5(7) . . ? C4D C3D C31D 107.7(6) . . ? C4D C3D C2D 109.7(6) . . ? C31D C3D C2D 110.1(6) . . ? O5D C4D N21D 120.0(7) . . ? O5D C4D C3D 118.9(6) . . ? N21D C4D C3D 120.9(7) . . ? C4D N21D C23D 125.4(6) . . ? C4D N21D C22D 118.6(6) . . ? C23D N21D C22D 115.8(6) . . ? C4D O5D Nd2 126.1(5) . . ? C32D C31D C3D 112.5(7) . . ? O33D C32D C31D 114.2(7) . . ? C34D O33D C32D 116.2(8) . . ? O33D C34D C35D 109.1(10) . . ? C28D C23D C24D 117.9(9) . . ? C28D C23D N21D 121.5(9) . . ? C24D C23D N21D 120.4(7) . . ? C25D C24D C23D 121.6(9) . . ? C26D C25D C24D 119.2(11) . . ? C25D C26D C27D 121.0(12) . . ? C26D C27D C28D 120.1(12) . . ? C23D C28D C27D 120.1(11) . . ? C2D N11D C13D 127.9(7) . . ? C2D N11D C12D 117.1(7) . . ? C13D N11D C12D 115.0(7) . . ? C14D C13D C18D 121.7(10) . . ? C14D C13D N11D 119.6(9) . . ? C18D C13D N11D 118.6(9) . . ? C13D C14D C15D 118.2(13) . . ? C16D C15D C14D 121.0(16) . . ? C17D C16D C15D 120.0(16) . . ? C16D C17D C18D 119.6(18) . . ? C13D C18D C17D 119.4(14) . . ? _refine_diff_density_max 1.842 _refine_diff_density_min -1.659 _refine_diff_density_rms 0.101 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Pr(L4)2(NO3)3 _chemical_formula_sum 'C42 H52 N7 O15 Pr' _chemical_formula_weight 1039.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pr' 'Pr' -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 27.79(3) _cell_length_b 18.26(2) _cell_length_c 19.16(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.797(10) _cell_angle_gamma 90.00 _cell_volume 9631(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used all _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4260 _exptl_absorpt_coefficient_mu 1.084 _exptl_absorpt_correction_type 'DIFABS(Walker and Stuart, 1983)' _exptl_absorpt_correction_T_min 0.42 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Marresearch Image Plate' _diffrn_measurement_method '95 frames at 2^o intervals, counting time 2 min.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31539 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 26.15 _reflns_number_total 16889 _reflns_number_gt 10211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'XDS (Kabsch, 1991)' _computing_cell_refinement XDS _computing_data_reduction XDS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'PLATON(Spek,1994)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+99.9046P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000000(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 16889 _refine_ls_number_parameters 1184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1922 _refine_ls_R_factor_gt 0.1119 _refine_ls_wR_factor_ref 0.1745 _refine_ls_wR_factor_gt 0.1504 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _refine_ls_shift/su_max 0.085 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.24658(2) 0.82143(3) 0.24825(3) 0.03877(18) Uani 1 d . . . O51A O 0.3206(3) 0.7787(4) 0.3395(4) 0.054(2) Uani 1 d . . . N53A N 0.3461(3) 0.7583(5) 0.2922(6) 0.051(3) Uani 1 d . . . O52A O 0.3271(3) 0.7567(4) 0.2286(5) 0.059(2) Uani 1 d . . . O54A O 0.3896(3) 0.7408(6) 0.3084(5) 0.096(3) Uani 1 d . . . O61A O 0.2267(3) 0.7071(5) 0.1720(5) 0.064(2) Uani 1 d . . . N63A N 0.2277(4) 0.6610(6) 0.2235(6) 0.061(3) Uani 1 d . . . O62A O 0.2362(4) 0.6858(4) 0.2864(5) 0.073(3) Uani 1 d . . . O64A O 0.2178(4) 0.5953(5) 0.2123(6) 0.112(4) Uani 1 d . . . N73A N 0.1388(3) 0.8213(5) 0.1874(5) 0.053(2) Uani 1 d . . . O71A O 0.1534(3) 0.7980(5) 0.2509(5) 0.065(2) Uani 1 d . . . O72A O 0.1699(2) 0.8430(5) 0.1506(4) 0.068(3) Uani 1 d . . . O74A O 0.0959(3) 0.8201(8) 0.1652(6) 0.121(5) Uani 1 d . . . O1A O 0.2674(2) 0.8660(4) 0.1352(4) 0.0390(17) Uani 1 d . . . C2A C 0.3084(3) 0.8810(5) 0.1233(5) 0.025(2) Uani 1 d . . . C3A C 0.3336(3) 0.9515(5) 0.1512(5) 0.029(2) Uani 1 d . . . H3A H 0.3650 0.9562 0.1340 0.034 Uiso 1 calc R . . C4A C 0.3408(3) 0.9485(5) 0.2332(6) 0.036(2) Uani 1 d . . . O5A O 0.3144(3) 0.9118(4) 0.2663(4) 0.0463(18) Uani 1 d . . . C31A C 0.3009(4) 1.0175(6) 0.1267(6) 0.052(3) Uani 1 d . . . H31A H 0.2678 1.0077 0.1348 0.063 Uiso 1 calc R . . H31B H 0.3122 1.0606 0.1536 0.063 Uiso 1 calc R . . C32A C 0.3022(5) 1.0313(7) 0.0487(7) 0.066(4) Uani 1 d . . . H32A H 0.2934 0.9871 0.0220 0.079 Uiso 1 calc R . . H32B H 0.2792 1.0696 0.0320 0.079 Uiso 1 calc R . . O33A O 0.3492(3) 1.0527(5) 0.0397(5) 0.074(3) Uani 1 d . . . C34A C 0.3556(7) 1.0599(8) -0.0322(6) 0.092(6) Uani 1 d . . . H34A H 0.3353 1.0991 -0.0542 0.110 Uiso 1 calc R . . H34B H 0.3468 1.0147 -0.0573 0.110 Uiso 1 calc R . . C35A C 0.4062(7) 1.0762(11) -0.0337(9) 0.129(8) Uani 1 d . . . H35A H 0.4259 1.0423 -0.0039 0.155 Uiso 1 calc R . . H35B H 0.4129 1.1252 -0.0170 0.155 Uiso 1 calc R . . H35C H 0.4135 1.0720 -0.0811 0.155 Uiso 1 calc R . . N21A N 0.3758(4) 0.9909(5) 0.2683(5) 0.049(2) Uani 1 d . . . C22A C 0.3798(5) 0.9941(8) 0.3469(7) 0.084(5) Uani 1 d . . . H22A H 0.4118 1.0096 0.3660 0.101 Uiso 1 calc R . . H22B H 0.3736 0.9465 0.3650 0.101 Uiso 1 calc R . . H22C H 0.3564 1.0283 0.3602 0.101 Uiso 1 calc R . . C23A C 0.4077(3) 1.0381(6) 0.2360(6) 0.048(3) Uani 1 d . . . C24A C 0.4457(4) 1.0102(7) 0.2056(7) 0.063(4) Uani 1 d . . . H24A H 0.4502 0.9598 0.2045 0.076 Uiso 1 calc R . . C25A C 0.4775(5) 1.0558(9) 0.1764(9) 0.083(5) Uani 1 d . . . H25A H 0.5022 1.0362 0.1537 0.100 Uiso 1 calc R . . C26A C 0.4721(6) 1.1308(10) 0.1815(9) 0.095(5) Uani 1 d . . . H26A H 0.4937 1.1619 0.1633 0.114 Uiso 1 calc R . . C27A C 0.4350(5) 1.1594(8) 0.2133(8) 0.079(4) Uani 1 d . . . H27A H 0.4316 1.2099 0.2169 0.095 Uiso 1 calc R . . C28A C 0.4027(4) 1.1132(7) 0.2400(7) 0.063(4) Uani 1 d . . . H28A H 0.3773 1.1329 0.2609 0.076 Uiso 1 calc R . . N11A N 0.3322(3) 0.8369(5) 0.0826(5) 0.042(2) Uani 1 d . . . C12A C 0.3074(5) 0.7712(8) 0.0518(8) 0.093(6) Uani 1 d . . . H12A H 0.3221 0.7283 0.0748 0.112 Uiso 1 calc R . . H12B H 0.3102 0.7691 0.0024 0.112 Uiso 1 calc R . . H12C H 0.2738 0.7731 0.0580 0.112 Uiso 1 calc R . . C13A C 0.3823(4) 0.8441(6) 0.0724(6) 0.071(3) Uani 1 d . . . C14A C 0.3941(5) 0.8630(8) 0.0056(7) 0.077(4) Uani 1 d . . . H14A H 0.3698 0.8769 -0.0304 0.093 Uiso 1 calc R . . C15A C 0.4417(6) 0.8607(11) -0.0059(9) 0.110(6) Uani 1 d . . . H15A H 0.4504 0.8727 -0.0497 0.131 Uiso 1 calc R . . C16A C 0.4765(6) 0.8402(11) 0.0492(11) 0.109(6) Uani 1 d . . . H16A H 0.5088 0.8389 0.0415 0.131 Uiso 1 calc R . . C17A C 0.4656(5) 0.8217(8) 0.1147(8) 0.082(5) Uani 1 d . . . H17A H 0.4902 0.8092 0.1507 0.099 Uiso 1 calc R . . C18A C 0.4185(4) 0.8220(7) 0.1262(6) 0.057(3) Uani 1 d . . . H18A H 0.4103 0.8075 0.1696 0.068 Uiso 1 calc R . . O1B O 0.2124(3) 0.9435(4) 0.2666(4) 0.053(2) Uani 1 d . . . C2B C 0.1768(4) 0.9631(6) 0.2956(7) 0.055(3) Uani 1 d . . . C3B C 0.1762(4) 0.9424(6) 0.3741(6) 0.045(3) Uani 1 d . . . H3B H 0.1446 0.9544 0.3883 0.054 Uiso 1 calc R . . C4B C 0.1869(4) 0.8602(5) 0.3852(6) 0.040(3) Uani 1 d . . . O5B O 0.2240(2) 0.8334(4) 0.3694(4) 0.0457(18) Uani 1 d . . . C31B C 0.2179(4) 0.9863(6) 0.4207(7) 0.059(3) Uani 1 d . . . H31C H 0.2194 0.9701 0.4692 0.071 Uiso 1 calc R . . H31D H 0.2487 0.9743 0.4051 0.071 Uiso 1 calc R . . C32B C 0.2115(5) 1.0670(7) 0.4185(8) 0.071(4) Uani 1 d . . . H32C H 0.2378 1.0895 0.4496 0.085 Uiso 1 calc R . . H32D H 0.2133 1.0843 0.3711 0.085 Uiso 1 calc R . . O33B O 0.1657(4) 1.0888(5) 0.4396(5) 0.074(3) Uani 1 d . . . C34B C 0.1644(6) 1.0904(9) 0.5126(9) 0.091(5) Uani 1 d . . . H34C H 0.1897 1.1223 0.5353 0.109 Uiso 1 calc R . . H34D H 0.1697 1.0416 0.5322 0.109 Uiso 1 calc R . . C35B C 0.1151(7) 1.1184(9) 0.5246(9) 0.113(6) Uani 1 d . . . H35D H 0.1110 1.1115 0.5731 0.136 Uiso 1 calc R . . H35E H 0.0904 1.0919 0.4952 0.136 Uiso 1 calc R . . H35F H 0.1126 1.1696 0.5132 0.136 Uiso 1 calc R . . N11B N 0.1410(4) 1.0019(5) 0.2622(6) 0.063(3) Uani 1 d . . . C12B C 0.1485(7) 1.0270(8) 0.1888(8) 0.115(7) Uani 1 d . . . H12D H 0.1500 1.0796 0.1877 0.138 Uiso 1 calc R . . H12E H 0.1220 1.0104 0.1553 0.138 Uiso 1 calc R . . H12F H 0.1784 1.0071 0.1772 0.138 Uiso 1 calc R . . C13B C 0.0972(4) 1.0223(7) 0.2856(7) 0.058(3) Uani 1 d . . . C14B C 0.0892(5) 1.0928(8) 0.3054(8) 0.078(4) Uani 1 d . . . H14B H 0.1132 1.1281 0.3047 0.094 Uiso 1 calc R . . C15B C 0.0450(8) 1.1110(11) 0.3265(9) 0.109(7) Uani 1 d . . . H15B H 0.0398 1.1581 0.3423 0.130 Uiso 1 calc R . . C16B C 0.0088(7) 1.0595(13) 0.3242(9) 0.112(7) Uani 1 d . . . H16B H -0.0213 1.0727 0.3363 0.134 Uiso 1 calc R . . C17B C 0.0168(6) 0.9884(11) 0.3042(8) 0.095(5) Uani 1 d . . . H17B H -0.0076 0.9533 0.3027 0.114 Uiso 1 calc R . . C18B C 0.0614(5) 0.9707(8) 0.2864(8) 0.077(4) Uani 1 d . . . H18B H 0.0677 0.9225 0.2745 0.093 Uiso 1 calc R . . N21B N 0.1550(3) 0.8219(5) 0.4172(5) 0.042(2) Uani 1 d . . . C22B C 0.1644(5) 0.7414(6) 0.4253(8) 0.070(4) Uani 1 d . . . H22D H 0.1681 0.7286 0.4743 0.084 Uiso 1 calc R . . H22E H 0.1936 0.7292 0.4061 0.084 Uiso 1 calc R . . H22F H 0.1376 0.7149 0.4005 0.084 Uiso 1 calc R . . C23B C 0.1120(4) 0.8485(6) 0.4423(6) 0.050(3) Uani 1 d . . . C24B C 0.1169(5) 0.8946(7) 0.5023(6) 0.062(4) Uani 1 d . . . H24B H 0.1474 0.9080 0.5249 0.075 Uiso 1 calc R . . C25B C 0.0753(6) 0.9186(7) 0.5257(7) 0.075(4) Uani 1 d . . . H25B H 0.0777 0.9509 0.5635 0.089 Uiso 1 calc R . . C26B C 0.0318(6) 0.8974(9) 0.4962(10) 0.092(5) Uani 1 d . . . H26B H 0.0045 0.9135 0.5151 0.111 Uiso 1 calc R . . C27B C 0.0256(6) 0.8519(10) 0.4378(11) 0.114(7) Uani 1 d . . . H27B H -0.0051 0.8373 0.4170 0.136 Uiso 1 calc R . . C28B C 0.0681(5) 0.8287(9) 0.4114(9) 0.091(5) Uani 1 d . . . H28B H 0.0655 0.7990 0.3716 0.109 Uiso 1 calc R . . Pr2 Pr 0.24591(2) 0.93540(3) 0.74899(3) 0.03957(19) Uani 1 d . . . N53C N 0.3535(3) 0.9336(6) 0.8038(7) 0.069(4) Uani 1 d . . . O52C O 0.3228(3) 0.9084(5) 0.8441(5) 0.060(2) Uani 1 d . . . O54C O 0.3976(3) 0.9291(7) 0.8277(6) 0.104(4) Uani 1 d . . . O51C O 0.3376(3) 0.9560(5) 0.7431(4) 0.055(2) Uani 1 d . . . O62C O 0.1738(3) 0.9817(4) 0.6578(4) 0.058(2) Uani 1 d . . . N63C N 0.1468(4) 1.0012(6) 0.7022(6) 0.059(3) Uani 1 d . . . O61C O 0.1661(3) 1.0006(4) 0.7665(4) 0.057(2) Uani 1 d . . . O64C O 0.1054(3) 1.0234(7) 0.6850(6) 0.103(4) Uani 1 d . . . O71C O 0.2688(3) 1.0468(5) 0.8277(5) 0.067(2) Uani 1 d . . . O74C O 0.2863(4) 1.1545(5) 0.7923(6) 0.096(3) Uani 1 d . . . N73C N 0.2719(4) 1.0925(6) 0.7804(7) 0.066(3) Uani 1 d . . . O72C O 0.2607(3) 1.0708(4) 0.7162(5) 0.070(3) Uani 1 d . . . O1C O 0.1780(3) 0.8447(4) 0.7281(4) 0.0490(19) Uani 1 d . . . C2C C 0.1508(4) 0.8052(6) 0.7605(6) 0.041(3) Uani 1 d . . . C3C C 0.1585(4) 0.8026(5) 0.8396(6) 0.042(3) Uani 1 d . . . H3C H 0.1270 0.7949 0.8561 0.050 Uiso 1 calc R . . C4C C 0.1805(3) 0.8738(5) 0.8718(5) 0.034(2) Uani 1 d . . . O5C O 0.2228(2) 0.8895(4) 0.8604(4) 0.0432(18) Uani 1 d . . . C31C C 0.1924(4) 0.7383(6) 0.8658(6) 0.053(3) Uani 1 d . . . H31E H 0.1817 0.6948 0.8391 0.064 Uiso 1 calc R . . H31F H 0.2250 0.7495 0.8563 0.064 Uiso 1 calc R . . C32C C 0.1941(4) 0.7219(7) 0.9422(7) 0.065(4) Uani 1 d . . . H32E H 0.2181 0.6844 0.9564 0.077 Uiso 1 calc R . . H32F H 0.2028 0.7656 0.9698 0.077 Uiso 1 calc R . . O33C O 0.1482(3) 0.6979(5) 0.9529(4) 0.061(2) Uani 1 d . . . C34C C 0.1433(6) 0.6885(8) 1.0262(8) 0.081(5) Uani 1 d . . . H34E H 0.1512 0.7339 1.0514 0.097 Uiso 1 calc R . . H34F H 0.1656 0.6509 1.0467 0.097 Uiso 1 calc R . . C35C C 0.0922(7) 0.6668(10) 1.0325(10) 0.120(7) Uani 1 d . . . H35G H 0.0885 0.6618 1.0814 0.144 Uiso 1 calc R . . H35H H 0.0850 0.6209 1.0090 0.144 Uiso 1 calc R . . H35I H 0.0703 0.7037 1.0113 0.144 Uiso 1 calc R . . N11C N 0.1169(3) 0.7644(5) 0.7236(5) 0.045(2) Uani 1 d . . . C12C C 0.1134(5) 0.7622(7) 0.6482(6) 0.074(4) Uani 1 d . . . H12G H 0.1031 0.8091 0.6291 0.089 Uiso 1 calc R . . H12H H 0.0903 0.7256 0.6301 0.089 Uiso 1 calc R . . H12I H 0.1446 0.7503 0.6349 0.089 Uiso 1 calc R . . C13C C 0.0844(4) 0.7171(6) 0.7561(6) 0.045(3) Uani 1 d . . . C14C C 0.0460(4) 0.7445(8) 0.7839(7) 0.069(4) Uani 1 d . . . H14C H 0.0411 0.7949 0.7842 0.083 Uiso 1 calc R . . C15C C 0.0131(5) 0.6978(11) 0.8126(9) 0.094(6) Uani 1 d . . . H15C H -0.0134 0.7162 0.8317 0.113 Uiso 1 calc R . . C16C C 0.0224(6) 0.6238(11) 0.8108(8) 0.091(6) Uani 1 d . . . H16C H 0.0024 0.5920 0.8316 0.109 Uiso 1 calc R . . C17C C 0.0598(6) 0.5949(8) 0.7796(9) 0.092(6) Uani 1 d . . . H17C H 0.0636 0.5444 0.7765 0.110 Uiso 1 calc R . . C18C C 0.0916(5) 0.6413(7) 0.7532(7) 0.066(4) Uani 1 d . . . H18C H 0.1178 0.6225 0.7333 0.079 Uiso 1 calc R . . N21C N 0.1567(4) 0.9164(5) 0.9119(6) 0.059(3) Uani 1 d . . . C22C C 0.1813(5) 0.9835(7) 0.9439(8) 0.087(5) Uani 1 d . . . H22G H 0.1834 0.9808 0.9943 0.105 Uiso 1 calc R . . H22H H 0.1630 1.0261 0.9271 0.105 Uiso 1 calc R . . H22I H 0.2135 0.9865 0.9310 0.105 Uiso 1 calc R . . C23C C 0.1070(4) 0.9056(6) 0.9193(6) 0.049(3) Uani 1 d . . . C24C C 0.0704(5) 0.9280(7) 0.8662(7) 0.068(4) Uani 1 d . . . H24C H 0.0786 0.9463 0.8241 0.081 Uiso 1 calc R . . C25C C 0.0224(5) 0.9232(10) 0.8757(10) 0.101(6) Uani 1 d . . . H25C H -0.0024 0.9360 0.8401 0.122 Uiso 1 calc R . . C26C C 0.0125(7) 0.8987(13) 0.9398(12) 0.130(8) Uani 1 d . . . H26C H -0.0199 0.8961 0.9471 0.156 Uiso 1 calc R . . C27C C 0.0465(8) 0.8783(12) 0.9927(12) 0.141(9) Uani 1 d . . . H27C H 0.0379 0.8613 1.0351 0.169 Uiso 1 calc R . . C28C C 0.0953(6) 0.8832(9) 0.9825(8) 0.096(6) Uani 1 d . . . H28C H 0.1197 0.8711 1.0189 0.115 Uiso 1 calc R . . O1D O 0.2790(3) 0.8143(4) 0.7285(4) 0.052(2) Uani 1 d . . . C2D C 0.3134(4) 0.7948(5) 0.6987(6) 0.040(3) Uani 1 d . . . C3D C 0.3136(4) 0.8163(6) 0.6201(6) 0.045(3) Uani 1 d . . . H3D H 0.3450 0.8037 0.6053 0.054 Uiso 1 calc R . . C4D C 0.3036(4) 0.8968(6) 0.6090(5) 0.044(3) Uani 1 d . . . N21D N 0.3338(3) 0.9391(5) 0.5791(5) 0.044(2) Uani 1 d . . . O5D O 0.2663(3) 0.9238(4) 0.6281(4) 0.0462(19) Uani 1 d . . . C31D C 0.2718(4) 0.7735(5) 0.5741(6) 0.051(3) Uani 1 d . . . H31G H 0.2414 0.7837 0.5918 0.061 Uiso 1 calc R . . H31H H 0.2689 0.7916 0.5261 0.061 Uiso 1 calc R . . C32D C 0.2793(5) 0.6916(7) 0.5734(8) 0.074(4) Uani 1 d . . . H32G H 0.2774 0.6726 0.6202 0.088 Uiso 1 calc R . . H32H H 0.2530 0.6699 0.5416 0.088 Uiso 1 calc R . . O33D O 0.3236(4) 0.6698(5) 0.5526(5) 0.078(3) Uani 1 d . . . C34D C 0.3280(6) 0.6707(8) 0.4814(7) 0.088(5) Uani 1 d . . . H34G H 0.3212 0.7196 0.4627 0.106 Uiso 1 calc R . . H34H H 0.3045 0.6375 0.4564 0.106 Uiso 1 calc R . . C35D C 0.3778(7) 0.6485(10) 0.4701(9) 0.122(7) Uani 1 d . . . H35J H 0.3846 0.6672 0.4257 0.146 Uiso 1 calc R . . H35K H 0.3800 0.5960 0.4700 0.146 Uiso 1 calc R . . H35L H 0.4009 0.6678 0.5073 0.146 Uiso 1 calc R . . C22D C 0.3246(5) 1.0186(7) 0.5723(8) 0.076(4) Uani 1 d . . . H22J H 0.2906 1.0270 0.5577 0.091 Uiso 1 calc R . . H22K H 0.3429 1.0386 0.5378 0.091 Uiso 1 calc R . . H22L H 0.3342 1.0419 0.6169 0.091 Uiso 1 calc R . . C23D C 0.3773(4) 0.9148(7) 0.5525(7) 0.054(3) Uani 1 d . . . C24D C 0.3741(5) 0.8694(7) 0.4927(7) 0.059(3) Uani 1 d . . . H24D H 0.3438 0.8548 0.4705 0.071 Uiso 1 calc R . . C25D C 0.4151(6) 0.8466(8) 0.4671(8) 0.085(5) Uani 1 d . . . H25D H 0.4127 0.8144 0.4292 0.102 Uiso 1 calc R . . C26D C 0.4589(7) 0.8706(13) 0.4968(13) 0.136(8) Uani 1 d . . . H26D H 0.4865 0.8545 0.4787 0.163 Uiso 1 calc R . . C27D C 0.4641(6) 0.9180(14) 0.5528(13) 0.149(10) Uani 1 d . . . H27D H 0.4945 0.9356 0.5718 0.179 Uiso 1 calc R . . C28D C 0.4213(6) 0.9392(10) 0.5808(10) 0.122(7) Uani 1 d . . . H28D H 0.4238 0.9706 0.6193 0.146 Uiso 1 calc R . . N11D N 0.3487(3) 0.7525(5) 0.7288(5) 0.056(3) Uani 1 d . . . C13D C 0.3923(5) 0.7315(8) 0.7023(7) 0.068(4) Uani 1 d . . . C12D C 0.3448(6) 0.7272(8) 0.8018(7) 0.095(5) Uani 1 d . . . H12J H 0.3634 0.6830 0.8114 0.114 Uiso 1 calc R . . H12K H 0.3113 0.7177 0.8062 0.114 Uiso 1 calc R . . H12L H 0.3571 0.7644 0.8348 0.114 Uiso 1 calc R . . C14D C 0.3995(6) 0.6586(8) 0.6870(8) 0.087(5) Uani 1 d . . . H14D H 0.3756 0.6239 0.6916 0.104 Uiso 1 calc R . . C15D C 0.4430(10) 0.6385(14) 0.6646(12) 0.147(10) Uani 1 d . . . H15D H 0.4485 0.5899 0.6536 0.176 Uiso 1 calc R . . C16D C 0.4771(8) 0.689(2) 0.6589(15) 0.165(16) Uani 1 d . . . H16D H 0.5067 0.6744 0.6463 0.198 Uiso 1 calc R . . C17D C 0.4698(7) 0.7622(17) 0.6709(12) 0.153(11) Uani 1 d . . . H17D H 0.4933 0.7965 0.6638 0.184 Uiso 1 calc R . . C18D C 0.4267(6) 0.7840(11) 0.6939(9) 0.102(6) Uani 1 d . . . H18D H 0.4211 0.8330 0.7035 0.123 Uiso 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pr1 0.0378(4) 0.0399(4) 0.0391(4) 0.0033(3) 0.0070(3) 0.0002(2) O51A 0.057(5) 0.077(6) 0.027(5) 0.017(4) 0.004(4) 0.004(4) N53A 0.049(6) 0.047(6) 0.056(8) 0.014(5) 0.001(5) 0.007(4) O52A 0.064(5) 0.062(6) 0.046(6) 0.005(4) -0.006(4) 0.013(4) O54A 0.053(6) 0.157(10) 0.071(7) 0.006(7) -0.014(5) 0.032(6) O61A 0.076(6) 0.067(6) 0.042(6) -0.010(4) -0.011(4) 0.000(4) N63A 0.063(7) 0.062(8) 0.066(9) -0.022(6) 0.032(6) 0.001(5) O62A 0.115(8) 0.047(6) 0.061(7) 0.000(4) 0.032(6) -0.010(5) O64A 0.160(11) 0.051(7) 0.137(11) -0.055(6) 0.061(8) -0.041(6) N73A 0.041(5) 0.081(7) 0.035(6) -0.006(5) 0.003(5) 0.009(5) O71A 0.047(5) 0.098(7) 0.049(6) 0.008(5) 0.001(4) -0.020(4) O72A 0.026(4) 0.127(8) 0.051(6) 0.016(5) 0.008(4) 0.005(4) O74A 0.030(5) 0.235(15) 0.095(9) 0.002(9) -0.009(5) -0.004(7) O1A 0.022(3) 0.059(5) 0.035(5) 0.006(3) -0.002(3) -0.004(3) C2A 0.031(5) 0.027(5) 0.016(5) 0.004(4) 0.003(4) 0.010(4) C3A 0.044(5) 0.028(5) 0.016(6) 0.002(4) 0.013(4) -0.001(4) C4A 0.033(5) 0.027(6) 0.048(7) 0.000(5) 0.002(5) -0.005(4) O5A 0.061(5) 0.039(4) 0.040(5) 0.006(3) 0.008(4) -0.014(3) C31A 0.058(7) 0.023(6) 0.073(10) 0.007(5) -0.005(6) 0.011(5) C32A 0.087(10) 0.049(8) 0.054(9) 0.021(6) -0.022(7) -0.003(6) O33A 0.091(7) 0.073(7) 0.054(7) 0.017(5) -0.002(5) -0.031(5) C34A 0.186(18) 0.082(11) 0.009(8) 0.017(6) 0.015(9) -0.025(10) C35A 0.167(19) 0.155(19) 0.077(14) 0.014(12) 0.063(13) -0.041(15) N21A 0.083(7) 0.042(6) 0.020(6) 0.008(4) -0.001(5) -0.014(5) C22A 0.110(12) 0.084(11) 0.050(10) 0.004(7) -0.012(8) -0.024(8) C23A 0.026(5) 0.050(8) 0.067(9) 0.012(6) -0.001(5) -0.006(4) C24A 0.052(7) 0.055(8) 0.078(10) 0.001(7) -0.012(7) -0.007(6) C25A 0.050(8) 0.098(13) 0.104(14) -0.020(10) 0.023(8) -0.015(8) C26A 0.083(12) 0.093(14) 0.106(15) 0.024(10) 0.005(10) -0.031(9) C27A 0.075(10) 0.052(9) 0.108(13) 0.011(8) 0.000(9) -0.018(7) C28A 0.064(8) 0.053(9) 0.073(10) 0.007(7) 0.011(7) -0.001(6) N11A 0.035(5) 0.047(6) 0.045(6) -0.016(4) 0.002(4) -0.005(4) C12A 0.087(10) 0.090(12) 0.106(14) -0.072(10) 0.023(9) -0.027(8) C13A 0.074(8) 0.057(7) 0.083(10) 0.003(6) 0.013(7) 0.004(5) C14A 0.083(10) 0.128(13) 0.026(8) 0.018(8) 0.022(7) 0.011(8) C15A 0.089(12) 0.181(19) 0.066(12) 0.031(12) 0.038(10) 0.030(12) C16A 0.074(11) 0.158(17) 0.104(16) 0.009(13) 0.049(11) 0.009(11) C17A 0.050(8) 0.115(13) 0.075(12) 0.004(9) -0.014(7) 0.024(8) C18A 0.049(7) 0.076(9) 0.041(8) 0.008(6) -0.007(6) 0.020(6) O1B 0.066(5) 0.041(5) 0.057(6) 0.012(4) 0.023(4) 0.010(4) C2B 0.047(7) 0.039(7) 0.086(10) -0.002(6) 0.031(7) 0.009(5) C3B 0.043(6) 0.052(7) 0.043(8) -0.003(5) 0.017(5) -0.019(5) C4B 0.041(6) 0.034(7) 0.041(8) -0.007(5) -0.011(5) -0.004(4) O5B 0.039(4) 0.064(5) 0.035(5) 0.004(4) 0.006(3) 0.011(3) C31B 0.060(8) 0.053(9) 0.063(9) -0.012(6) 0.004(6) -0.006(6) C32B 0.092(10) 0.055(9) 0.065(10) -0.008(7) 0.008(8) -0.016(7) O33B 0.103(8) 0.056(6) 0.059(7) -0.015(5) 0.002(5) 0.003(5) C34B 0.098(12) 0.096(13) 0.079(14) 0.005(9) 0.009(10) -0.015(9) C35B 0.168(19) 0.097(14) 0.086(14) -0.016(10) 0.059(13) -0.018(12) N11B 0.080(7) 0.055(7) 0.059(8) 0.020(5) 0.028(6) 0.026(5) C12B 0.170(17) 0.091(13) 0.093(14) 0.062(10) 0.050(12) 0.074(11) C13B 0.058(8) 0.072(10) 0.047(9) 0.000(6) 0.013(6) 0.016(6) C14B 0.087(10) 0.062(10) 0.077(11) -0.006(8) -0.018(8) 0.021(7) C15B 0.131(17) 0.108(16) 0.083(14) -0.016(11) -0.001(12) 0.070(13) C16B 0.099(14) 0.17(2) 0.064(12) 0.005(13) 0.021(11) 0.070(14) C17B 0.079(11) 0.125(16) 0.080(13) 0.010(11) 0.008(9) 0.000(10) C18B 0.075(10) 0.073(11) 0.084(12) 0.010(8) 0.014(8) 0.017(8) N21B 0.038(5) 0.051(6) 0.039(6) -0.006(4) 0.009(4) -0.009(4) C22B 0.076(9) 0.045(8) 0.090(12) 0.020(7) 0.020(8) 0.008(6) C23B 0.054(7) 0.055(8) 0.043(8) 0.001(6) 0.017(6) -0.002(5) C24B 0.094(10) 0.063(9) 0.036(8) 0.007(6) 0.031(7) -0.009(7) C25B 0.114(12) 0.064(10) 0.054(10) -0.002(7) 0.043(9) -0.003(8) C26B 0.069(10) 0.109(14) 0.110(15) 0.000(11) 0.050(10) -0.002(9) C27B 0.067(11) 0.111(15) 0.16(2) -0.037(13) 0.017(11) -0.019(9) C28B 0.060(9) 0.111(13) 0.096(13) -0.046(10) -0.008(8) -0.018(8) Pr2 0.0398(4) 0.0385(4) 0.0405(5) -0.0030(3) 0.0059(3) -0.0020(3) N53C 0.033(6) 0.084(9) 0.086(11) -0.026(7) -0.003(6) -0.005(5) O52C 0.043(5) 0.073(6) 0.058(6) -0.006(4) -0.012(4) -0.001(4) O54C 0.036(5) 0.180(12) 0.090(8) 0.008(7) -0.009(5) 0.000(6) O51C 0.041(4) 0.099(6) 0.020(4) 0.008(4) -0.009(3) -0.017(4) O62C 0.057(5) 0.067(6) 0.050(6) 0.007(4) 0.010(4) 0.015(4) N63C 0.051(6) 0.075(8) 0.051(8) 0.000(6) 0.001(5) 0.020(5) O61C 0.060(5) 0.070(6) 0.041(6) -0.001(4) 0.007(4) 0.016(4) O64C 0.056(6) 0.157(11) 0.089(8) -0.021(7) -0.011(5) 0.033(6) O71C 0.094(7) 0.042(6) 0.063(7) 0.002(4) 0.010(5) -0.012(4) O74C 0.123(9) 0.059(7) 0.109(9) -0.003(6) 0.022(7) -0.022(6) N73C 0.087(8) 0.037(7) 0.077(10) -0.012(6) 0.026(7) -0.014(5) O72C 0.093(7) 0.043(6) 0.081(8) -0.006(5) 0.031(6) -0.009(4) O1C 0.065(5) 0.051(5) 0.031(5) -0.001(3) 0.006(4) -0.018(4) C2C 0.038(6) 0.055(7) 0.030(7) -0.004(5) 0.005(5) 0.005(5) C3C 0.041(6) 0.035(6) 0.047(8) 0.008(5) -0.001(5) -0.002(4) C4C 0.026(5) 0.042(6) 0.032(7) 0.007(5) -0.005(4) -0.004(4) O5C 0.045(4) 0.044(5) 0.040(5) -0.004(3) 0.002(3) -0.008(3) C31C 0.052(7) 0.058(8) 0.049(8) 0.013(6) 0.004(6) 0.002(5) C32C 0.062(8) 0.054(9) 0.069(10) 0.023(7) -0.022(7) -0.007(6) O33C 0.086(6) 0.075(6) 0.018(5) 0.006(4) -0.007(4) -0.020(5) C34C 0.108(13) 0.067(10) 0.061(11) 0.006(7) -0.010(9) -0.006(8) C35C 0.140(17) 0.128(17) 0.099(16) 0.028(12) 0.035(13) -0.014(13) N11C 0.052(5) 0.050(6) 0.030(6) 0.006(4) -0.001(4) -0.018(4) C12C 0.105(11) 0.073(10) 0.044(9) -0.003(7) 0.009(7) -0.046(8) C13C 0.042(6) 0.062(8) 0.027(7) 0.006(5) -0.009(5) -0.019(5) C14C 0.058(8) 0.085(10) 0.064(10) -0.004(7) 0.011(7) -0.002(7) C15C 0.047(8) 0.146(16) 0.092(14) -0.030(11) 0.013(8) -0.037(9) C16C 0.104(13) 0.124(16) 0.044(10) 0.006(9) 0.007(9) -0.059(11) C17C 0.124(14) 0.064(11) 0.079(12) 0.024(8) -0.018(10) -0.054(10) C18C 0.083(9) 0.046(9) 0.063(10) 0.008(6) -0.013(7) -0.022(6) N21C 0.056(6) 0.063(7) 0.060(8) -0.021(5) 0.010(5) -0.004(5) C22C 0.111(12) 0.073(11) 0.082(12) -0.043(8) 0.025(9) -0.019(8) C23C 0.060(7) 0.045(7) 0.048(8) -0.005(5) 0.025(6) 0.006(5) C24C 0.069(9) 0.077(10) 0.053(9) 0.005(7) -0.003(7) 0.022(7) C25C 0.059(9) 0.156(17) 0.089(14) 0.016(11) 0.010(9) 0.033(9) C26C 0.081(13) 0.20(2) 0.119(19) 0.023(16) 0.057(13) 0.028(13) C27C 0.145(19) 0.19(2) 0.107(18) 0.060(16) 0.083(15) 0.053(17) C28C 0.093(12) 0.132(15) 0.068(12) 0.036(10) 0.025(9) 0.041(10) O1D 0.067(5) 0.043(5) 0.050(5) 0.011(4) 0.023(4) 0.014(4) C2D 0.057(7) 0.013(5) 0.048(8) -0.005(4) -0.002(5) 0.009(4) C3D 0.046(6) 0.042(7) 0.045(8) -0.004(5) 0.000(5) 0.002(5) C4D 0.061(7) 0.053(8) 0.014(6) 0.014(5) -0.007(5) -0.006(5) N21D 0.058(6) 0.043(6) 0.032(6) -0.001(4) 0.012(4) 0.003(4) O5D 0.048(4) 0.057(5) 0.036(5) 0.000(3) 0.014(3) 0.013(3) C31D 0.051(7) 0.034(7) 0.069(9) -0.021(5) 0.011(6) -0.001(5) C32D 0.099(11) 0.046(9) 0.079(11) -0.010(7) 0.025(9) -0.012(7) O33D 0.122(8) 0.065(6) 0.048(6) -0.008(5) 0.016(6) 0.022(5) C34D 0.140(15) 0.087(12) 0.043(10) 0.004(8) 0.032(9) -0.023(10) C35D 0.165(18) 0.115(15) 0.103(15) -0.015(11) 0.083(14) 0.003(13) C22D 0.096(11) 0.053(9) 0.085(12) 0.009(7) 0.031(9) 0.007(7) C23D 0.053(7) 0.053(8) 0.054(9) 0.020(6) 0.006(6) -0.011(5) C24D 0.063(8) 0.064(9) 0.051(9) 0.005(6) 0.013(7) -0.005(6) C25D 0.120(13) 0.086(11) 0.055(10) 0.015(8) 0.038(9) 0.008(9) C26D 0.081(13) 0.16(2) 0.18(3) -0.023(17) 0.048(15) -0.032(13) C27D 0.060(11) 0.21(3) 0.18(3) -0.039(19) 0.009(13) -0.056(13) C28D 0.075(11) 0.157(18) 0.136(18) -0.072(14) 0.021(11) -0.043(11) N11D 0.060(6) 0.064(7) 0.048(7) 0.012(5) 0.024(5) 0.014(5) C13D 0.067(9) 0.095(11) 0.039(8) 0.012(7) -0.006(6) 0.024(8) C12D 0.130(13) 0.096(12) 0.064(11) 0.028(9) 0.030(10) 0.061(10) C14D 0.105(12) 0.066(11) 0.092(13) 0.010(8) 0.021(9) 0.039(8) C15D 0.18(2) 0.14(2) 0.121(19) -0.007(16) 0.018(19) 0.112(19) C16D 0.070(14) 0.31(5) 0.11(2) -0.06(3) -0.002(13) 0.07(2) C17D 0.072(14) 0.27(4) 0.111(19) -0.04(2) 0.002(12) -0.032(17) C18D 0.068(10) 0.144(17) 0.097(14) -0.016(12) 0.020(9) -0.008(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pr1 O1A 2.456(7) . ? Pr1 O1B 2.466(7) . ? Pr1 O5A 2.495(7) . ? Pr1 O5B 2.494(7) . ? Pr1 O61A 2.567(8) . ? Pr1 O52A 2.601(8) . ? Pr1 O62A 2.609(8) . ? Pr1 O51A 2.629(8) . ? Pr1 O71A 2.633(8) . ? Pr1 O72A 2.667(8) . ? O51A N53A 1.279(11) . ? N53A O54A 1.246(11) . ? N53A O52A 1.261(12) . ? O61A N63A 1.293(13) . ? N63A O64A 1.243(13) . ? N63A O62A 1.280(13) . ? N73A O74A 1.210(11) . ? N73A O72A 1.249(11) . ? N73A O71A 1.301(12) . ? O1A C2A 1.222(10) . ? C2A N11A 1.354(11) . ? C2A C3A 1.528(12) . ? C3A C31A 1.541(12) . ? C3A C4A 1.556(14) . ? C4A O5A 1.233(11) . ? C4A N21A 1.349(12) . ? C31A C32A 1.521(16) . ? C32A O33A 1.397(15) . ? O33A C34A 1.419(14) . ? C34A C35A 1.44(2) . ? N21A C23A 1.438(13) . ? N21A C22A 1.497(15) . ? C23A C24A 1.370(16) . ? C23A C28A 1.381(16) . ? C24A C25A 1.387(18) . ? C25A C26A 1.38(2) . ? C26A C27A 1.37(2) . ? C27A C28A 1.380(17) . ? N11A C13A 1.437(13) . ? N11A C12A 1.469(13) . ? C13A C18A 1.397(15) . ? C13A C14A 1.407(15) . ? C14A C15A 1.371(19) . ? C15A C16A 1.38(2) . ? C16A C17A 1.37(2) . ? C17A C18A 1.358(17) . ? O1B C2B 1.249(12) . ? C2B N11B 1.315(14) . ? C2B C3B 1.552(16) . ? C3B C4B 1.538(14) . ? C3B C31B 1.583(14) . ? C4B O5B 1.215(12) . ? C4B N21B 1.343(13) . ? C31B C32B 1.483(16) . ? C32B O33B 1.442(15) . ? O33B C34B 1.404(17) . ? C34B C35B 1.51(2) . ? N11B C13B 1.401(14) . ? N11B C12B 1.520(16) . ? C13B C18B 1.373(18) . ? C13B C14B 1.368(17) . ? C14B C15B 1.38(2) . ? C15B C16B 1.37(3) . ? C16B C17B 1.38(2) . ? C17B C18B 1.369(19) . ? N21B C23B 1.431(13) . ? N21B C22B 1.497(13) . ? C23B C28B 1.332(16) . ? C23B C24B 1.415(16) . ? C24B C25B 1.367(17) . ? C25B C26B 1.32(2) . ? C26B C27B 1.39(2) . ? C27B C28B 1.41(2) . ? Pr2 O1D 2.445(7) . ? Pr2 O5C 2.458(7) . ? Pr2 O5D 2.467(7) . ? Pr2 O1C 2.504(7) . ? Pr2 O71C 2.563(9) . ? Pr2 O61C 2.576(8) . ? Pr2 O51C 2.594(8) . ? Pr2 O72C 2.598(8) . ? Pr2 O62C 2.612(8) . ? Pr2 O52C 2.657(8) . ? N53C O54C 1.252(12) . ? O51C N53C 1.253(14) . ? N53C O52C 1.309(13) . ? O62C N63C 1.260(11) . ? N63C O64C 1.220(12) . ? N63C O61C 1.276(12) . ? O71C N73C 1.243(13) . ? O74C N73C 1.212(13) . ? N73C O72C 1.290(13) . ? O1C C2C 1.268(12) . ? C2C N11C 1.329(13) . ? C2C C3C 1.503(15) . ? C3C C4C 1.532(14) . ? C3C C31C 1.544(14) . ? C4C O5C 1.257(11) . ? C4C N21C 1.331(13) . ? C31C C32C 1.487(16) . ? C32C O33C 1.390(13) . ? O33C C34C 1.438(15) . ? C34C C35C 1.50(2) . ? N11C C12C 1.435(14) . ? N11C C13C 1.450(12) . ? C13C C14C 1.352(16) . ? C13C C18C 1.400(16) . ? C14C C15C 1.414(19) . ? C15C C16C 1.38(2) . ? C16C C17C 1.37(2) . ? C17C C18C 1.370(17) . ? N21C C23C 1.420(14) . ? N21C C22C 1.496(15) . ? C23C C28C 1.358(17) . ? C23C C24C 1.399(16) . ? C24C C25C 1.373(18) . ? C25C C26C 1.37(2) . ? C26C C27C 1.34(2) . ? C27C C28C 1.40(2) . ? O1D C2D 1.232(12) . ? C2D N11D 1.316(13) . ? C2D C3D 1.556(15) . ? C3D C4D 1.505(15) . ? C3D C31D 1.570(14) . ? C4D O5D 1.246(13) . ? C4D N21D 1.326(13) . ? N21D C23D 1.444(14) . ? N21D C22D 1.476(14) . ? C31D C32D 1.508(15) . ? C32D O33D 1.402(15) . ? O33D C34D 1.387(15) . ? C34D C35D 1.48(2) . ? C23D C28D 1.346(18) . ? C23D C24D 1.408(17) . ? C24D C25D 1.363(17) . ? C25D C26D 1.35(2) . ? C26D C27D 1.37(3) . ? C27D C28D 1.42(2) . ? N11D C13D 1.427(15) . ? N11D C12D 1.492(15) . ? C13D C18D 1.38(2) . ? C13D C14D 1.383(19) . ? C14D C15D 1.39(2) . ? C15D C16D 1.34(3) . ? C16D C17D 1.37(3) . ? C17D C18D 1.39(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Pr1 O1B 88.2(2) . . ? O1A Pr1 O5A 68.8(2) . . ? O1B Pr1 O5A 71.3(3) . . ? O1A Pr1 O5B 155.6(2) . . ? O1B Pr1 O5B 68.7(2) . . ? O5A Pr1 O5B 95.4(2) . . ? O1A Pr1 O61A 80.0(3) . . ? O1B Pr1 O61A 139.4(3) . . ? O5A Pr1 O61A 136.0(3) . . ? O5B Pr1 O61A 122.6(3) . . ? O1A Pr1 O52A 73.3(2) . . ? O1B Pr1 O52A 141.8(3) . . ? O5A Pr1 O52A 70.9(3) . . ? O5B Pr1 O52A 120.3(2) . . ? O61A Pr1 O52A 70.9(3) . . ? O1A Pr1 O62A 127.6(3) . . ? O1B Pr1 O62A 139.3(3) . . ? O5A Pr1 O62A 134.4(3) . . ? O5B Pr1 O62A 76.8(3) . . ? O61A Pr1 O62A 50.4(3) . . ? O52A Pr1 O62A 75.0(3) . . ? O1A Pr1 O51A 115.3(2) . . ? O1B Pr1 O51A 117.0(3) . . ? O5A Pr1 O51A 66.1(2) . . ? O5B Pr1 O51A 71.3(2) . . ? O61A Pr1 O51A 103.1(3) . . ? O52A Pr1 O51A 49.6(3) . . ? O62A Pr1 O51A 68.9(3) . . ? O1A Pr1 O71A 115.0(2) . . ? O1B Pr1 O71A 75.3(3) . . ? O5A Pr1 O71A 146.3(3) . . ? O5B Pr1 O71A 67.9(3) . . ? O61A Pr1 O71A 75.0(3) . . ? O52A Pr1 O71A 142.8(3) . . ? O62A Pr1 O71A 72.1(3) . . ? O51A Pr1 O71A 128.4(3) . . ? O1A Pr1 O72A 66.1(2) . . ? O1B Pr1 O72A 71.4(3) . . ? O5A Pr1 O72A 121.2(3) . . ? O5B Pr1 O72A 111.2(2) . . ? O61A Pr1 O72A 68.3(3) . . ? O52A Pr1 O72A 125.9(3) . . ? O62A Pr1 O72A 103.1(3) . . ? O51A Pr1 O72A 171.2(3) . . ? O71A Pr1 O72A 48.9(2) . . ? N53A O51A Pr1 94.2(6) . . ? O54A N53A O52A 119.9(10) . . ? O54A N53A O51A 120.6(11) . . ? O52A N53A O51A 119.4(9) . . ? N53A O52A Pr1 96.0(6) . . ? N63A O61A Pr1 96.6(7) . . ? O64A N63A O62A 120.9(12) . . ? O64A N63A O61A 120.9(12) . . ? O62A N63A O61A 118.1(11) . . ? N63A O62A Pr1 94.9(7) . . ? O74A N73A O72A 122.1(11) . . ? O74A N73A O71A 119.2(10) . . ? O72A N73A O71A 118.7(9) . . ? N73A O71A Pr1 96.3(6) . . ? N73A O72A Pr1 96.1(6) . . ? C2A O1A Pr1 125.2(6) . . ? O1A C2A N11A 120.9(9) . . ? O1A C2A C3A 121.2(8) . . ? N11A C2A C3A 117.9(8) . . ? C2A C3A C31A 109.2(8) . . ? C2A C3A C4A 108.4(7) . . ? C31A C3A C4A 109.0(8) . . ? O5A C4A N21A 119.8(10) . . ? O5A C4A C3A 122.2(9) . . ? N21A C4A C3A 117.9(8) . . ? C4A O5A Pr1 141.3(7) . . ? C32A C31A C3A 109.7(9) . . ? O33A C32A C31A 108.4(10) . . ? C32A O33A C34A 112.8(11) . . ? O33A C34A C35A 106.7(13) . . ? C4A N21A C23A 125.2(9) . . ? C4A N21A C22A 118.3(9) . . ? C23A N21A C22A 116.3(9) . . ? C24A C23A C28A 118.8(11) . . ? C24A C23A N21A 121.1(11) . . ? C28A C23A N21A 120.0(11) . . ? C23A C24A C25A 121.2(13) . . ? C26A C25A C24A 119.0(14) . . ? C27A C26A C25A 120.4(14) . . ? C26A C27A C28A 119.9(14) . . ? C23A C28A C27A 120.7(13) . . ? C2A N11A C13A 125.5(8) . . ? C2A N11A C12A 118.6(9) . . ? C13A N11A C12A 115.6(9) . . ? C18A C13A C14A 120.5(11) . . ? C18A C13A N11A 119.1(11) . . ? C14A C13A N11A 119.7(11) . . ? C15A C14A C13A 119.2(14) . . ? C14A C15A C16A 118.4(15) . . ? C17A C16A C15A 123.2(14) . . ? C18A C17A C16A 118.9(13) . . ? C17A C18A C13A 119.7(12) . . ? C2B O1B Pr1 131.7(7) . . ? O1B C2B N11B 122.0(12) . . ? O1B C2B C3B 118.3(10) . . ? N11B C2B C3B 119.7(9) . . ? C4B C3B C2B 110.1(9) . . ? C4B C3B C31B 107.7(9) . . ? C2B C3B C31B 108.7(9) . . ? O5B C4B N21B 122.6(10) . . ? O5B C4B C3B 120.8(10) . . ? N21B C4B C3B 116.4(9) . . ? C4B O5B Pr1 126.6(7) . . ? C32B C31B C3B 114.5(11) . . ? O33B C32B C31B 111.8(10) . . ? C34B O33B C32B 115.3(11) . . ? O33B C34B C35B 107.8(14) . . ? C2B N11B C13B 128.3(11) . . ? C2B N11B C12B 114.9(10) . . ? C13B N11B C12B 116.8(11) . . ? C18B C13B C14B 119.9(13) . . ? C18B C13B N11B 118.9(12) . . ? C14B C13B N11B 121.2(13) . . ? C13B C14B C15B 119.4(16) . . ? C16B C15B C14B 120.1(17) . . ? C15B C16B C17B 120.6(17) . . ? C18B C17B C16B 118.4(17) . . ? C17B C18B C13B 121.6(15) . . ? C4B N21B C23B 127.7(10) . . ? C4B N21B C22B 116.2(9) . . ? C23B N21B C22B 116.1(9) . . ? C28B C23B C24B 120.4(12) . . ? C28B C23B N21B 120.9(12) . . ? C24B C23B N21B 118.7(11) . . ? C25B C24B C23B 117.6(13) . . ? C26B C25B C24B 122.1(14) . . ? C25B C26B C27B 121.9(14) . . ? C26B C27B C28B 116.7(15) . . ? C23B C28B C27B 121.3(15) . . ? O1D Pr2 O5C 88.8(2) . . ? O1D Pr2 O5D 68.4(2) . . ? O5C Pr2 O5D 155.0(2) . . ? O1D Pr2 O1C 70.5(3) . . ? O5C Pr2 O1C 68.5(2) . . ? O5D Pr2 O1C 93.2(2) . . ? O1D Pr2 O71C 138.1(3) . . ? O5C Pr2 O71C 80.4(3) . . ? O5D Pr2 O71C 123.4(3) . . ? O1C Pr2 O71C 138.0(3) . . ? O1D Pr2 O61C 141.8(3) . . ? O5C Pr2 O61C 73.3(2) . . ? O5D Pr2 O61C 118.2(2) . . ? O1C Pr2 O61C 71.6(3) . . ? O71C Pr2 O61C 72.9(3) . . ? O1D Pr2 O51C 74.5(3) . . ? O5C Pr2 O51C 117.5(2) . . ? O5D Pr2 O51C 67.7(2) . . ? O1C Pr2 O51C 144.4(3) . . ? O71C Pr2 O51C 75.0(3) . . ? O61C Pr2 O51C 143.7(3) . . ? O1D Pr2 O72C 138.3(3) . . ? O5C Pr2 O72C 127.1(3) . . ? O5D Pr2 O72C 78.0(3) . . ? O1C Pr2 O72C 137.1(3) . . ? O71C Pr2 O72C 49.5(3) . . ? O61C Pr2 O72C 76.1(3) . . ? O51C Pr2 O72C 70.2(3) . . ? O1D Pr2 O62C 117.0(3) . . ? O5C Pr2 O62C 115.1(2) . . ? O5D Pr2 O62C 69.7(2) . . ? O1C Pr2 O62C 67.3(3) . . ? O71C Pr2 O62C 104.2(3) . . ? O61C Pr2 O62C 49.0(3) . . ? O51C Pr2 O62C 126.3(3) . . ? O72C Pr2 O62C 70.4(3) . . ? O1D Pr2 O52C 70.1(3) . . ? O5C Pr2 O52C 67.8(3) . . ? O5D Pr2 O52C 111.2(3) . . ? O1C Pr2 O52C 120.4(3) . . ? O71C Pr2 O52C 68.3(3) . . ? O61C Pr2 O52C 128.4(3) . . ? O51C Pr2 O52C 49.7(3) . . ? O72C Pr2 O52C 101.6(3) . . ? O62C Pr2 O52C 171.8(3) . . ? O54C N53C O51C 124.4(12) . . ? O54C N53C O52C 116.4(13) . . ? O51C N53C O52C 119.0(9) . . ? O51C O52C Pr2 93.4(7) . . ? N53C O51C Pr2 97.8(6) . . ? N63C O62C Pr2 96.4(7) . . ? O64C N63C O62C 122.4(11) . . ? O64C N63C O61C 121.4(10) . . ? O62C N63C O61C 116.0(9) . . ? N63C O61C Pr2 97.7(6) . . ? N73C O71C Pr2 98.1(8) . . ? O74C N73C O71C 123.0(13) . . ? O72C N73C O74C 119.9(12) . . ? O71C N73C O72C 117.1(11) . . ? N73C O72C Pr2 95.1(7) . . ? C2C O1C Pr2 141.8(7) . . ? O1C C2C N11C 119.2(10) . . ? O1C C2C C3C 119.9(9) . . ? N11C C2C C3C 120.9(9) . . ? C2C C3C C4C 112.0(8) . . ? C2C C3C C31C 110.4(9) . . ? C4C C3C C31C 108.8(8) . . ? O5C C4C N21C 121.1(10) . . ? O5C C4C C3C 117.2(9) . . ? N21C C4C C3C 121.7(9) . . ? C4C O5C Pr2 126.1(7) . . ? C32C C31C C3C 114.1(10) . . ? O33C C32C C31C 107.6(9) . . ? C32C O33C C34C 113.1(10) . . ? O33C C34C C35C 109.2(12) . . ? C2C N11C C12C 119.8(9) . . ? C2C N11C C13C 122.9(9) . . ? C12C N11C C13C 117.1(9) . . ? C14C C13C C18C 120.3(11) . . ? C14C C13C N11C 121.3(12) . . ? C18C C13C N11C 118.2(11) . . ? C13C C14C C15C 121.1(14) . . ? C16C C15C C14C 116.8(15) . . ? C17C C16C C15C 122.8(14) . . ? C18C C17C C16C 119.2(16) . . ? C17C C18C C13C 119.6(15) . . ? C4C N21C C23C 122.9(9) . . ? C4C N21C C22C 118.6(10) . . ? C23C N21C C22C 118.1(10) . . ? C28C C23C C24C 119.8(12) . . ? C28C C23C N21C 119.0(13) . . ? C24C C23C N21C 120.5(11) . . ? C25C C24C C23C 120.6(14) . . ? C26C C25C C24C 117.2(15) . . ? C27C C26C C25C 124.1(17) . . ? C26C C27C C28C 118.3(17) . . ? C23C C28C C27C 119.9(16) . . ? C2D O1D Pr2 131.9(7) . . ? O1D C2D N11D 123.1(11) . . ? O1D C2D C3D 118.7(9) . . ? N11D C2D C3D 118.1(9) . . ? C4D C3D C2D 111.0(9) . . ? C4D C3D C31D 107.5(9) . . ? C2D C3D C31D 108.5(9) . . ? O5D C4D N21D 119.9(10) . . ? O5D C4D C3D 119.1(10) . . ? N21D C4D C3D 121.0(11) . . ? C4D N21D C23D 125.7(10) . . ? C4D N21D C22D 119.9(10) . . ? C23D N21D C22D 114.4(9) . . ? C4D O5D Pr2 128.0(7) . . ? C32D C31D C3D 114.1(10) . . ? O33D C32D C31D 114.2(10) . . ? C34D O33D C32D 118.3(12) . . ? O33D C34D C35D 110.4(14) . . ? C28D C23D C24D 118.5(13) . . ? C28D C23D N21D 121.1(13) . . ? C24D C23D N21D 120.3(11) . . ? C25D C24D C23D 120.6(13) . . ? C26D C25D C24D 120.0(17) . . ? C25D C26D C27D 121.9(19) . . ? C26D C27D C28D 117.5(17) . . ? C23D C28D C27D 121.3(17) . . ? C2D N11D C13D 128.2(10) . . ? C2D N11D C12D 116.5(9) . . ? C13D N11D C12D 115.1(10) . . ? C18D C13D C14D 121.6(15) . . ? C18D C13D N11D 119.3(14) . . ? C14D C13D N11D 119.1(14) . . ? C13D C14D C15D 118.4(19) . . ? C16D C15D C14D 120(2) . . ? C15D C16D C17D 122(2) . . ? C16D C17D C18D 119(3) . . ? C13D C18D C17D 119(2) . . ? _refine_diff_density_max 1.541 _refine_diff_density_min -0.989 _refine_diff_density_rms 0.109 _publ_section_references ; Kabsch, W. (1988), J.Appl.Cryst 21 916-932. Sheldrick, G.M. (1990) SHELX86, Acta Cryst. A46 467-480. Sheldrick, G.M. (1993) SHELXL program for crystallography refinement. University of Gottingen, Germany. Spek, A.L., (1994) PLATON-94 program, Utrecht University, The Netherlands Walker, N. and Stuart, D., Acta Crystl 1983 A39 158. ; #====END